# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Wing-Tak, Wong' 'King-Fai, Li Billy' 'Kwok-Wai, Cheah' 'Po-Wan, Lai Winnie' _publ_contact_author_name 'Dr Wong Wing-Tak' _publ_contact_author_address ; Dept of Chemistry Overseas University of Hong Kong Pokfulam Road Hong Kong CHINA ; _publ_contact_author_email 'WTWONG@HKUCC.HKU.HK' _publ_section_title ; Synthesis, crystal structures, luminescence and magnetic properties of lanthanide complexes containing 1,8-bis(2-hydroxybenzamido)-3,6-dioxaoctane ligand ; data_wt0134w-Winnie027-complex_1 _database_code_CSD 175401 #------------------------------------------------------------------------------ _audit_creation_date 'Sat Sep 25 17:21:54 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 40.149(1) _cell_length_b 12.072(1) _cell_length_c 21.691(2) _cell_angle_alpha 90 _cell_angle_beta 91.97(2) _cell_angle_gamma 90 _cell_volume 10506(1) _cell_formula_units_Z 8 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c' 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' #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.260 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_meas ? _chemical_formula_weight 1152.40 _chemical_formula_analytical ? _chemical_formula_sum 'C22 H38 La2 N10 O27 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 4560.00 _exptl_absorpt_coefficient_mu 1.680 _exptl_absorpt_correction_type SAPABS #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'Bruker AXS SMART CCD' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 31479 _reflns_number_total 12448 _reflns_number_observed 6803 _reflns_observed_criterion 1.50 _diffrn_reflns_av_R_equivalents 0.04 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -51 _diffrn_reflns_limit_h_max 51 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.66 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source La 0 16 -0.287 2.452 'International Tables' C 0 176 0.003 0.002 'International Tables' N 0 80 0.006 0.003 'International Tables' O 0 216 0.011 0.006 'International Tables' H 0 304 0.000 0.000 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom La(1) 0.12482(2) 0.03524(7) -0.00134(3) 0.0416(2) Uij ? ? La(2) 0.11460(2) -0.29372(8) 0.04474(4) 0.0480(2) Uij ? ? O(1) 0.1853(2) -0.0010(8) -0.0047(4) 0.056(3) Uij ? ? O(2) 0.1364(2) -0.1577(7) -0.0322(3) 0.045(3) Uij ? ? O(3) 0.1150(2) -0.2284(8) 0.1540(4) 0.059(3) Uij ? ? O(4) 0.0924(2) -0.1047(7) 0.0535(3) 0.047(3) Uij ? ? O(5) 0.1560(3) 0.186(1) -0.0721(5) 0.082(4) Uij ? ? O(6) 0.1616(2) 0.2175(9) 0.0246(5) 0.065(4) Uij ? ? O(7) 0.1941(4) 0.302(1) -0.0363(7) 0.149(7) Uij ? ? O(8) 0.1131(2) 0.0322(8) -0.1225(4) 0.056(3) Uij ? ? O(9) 0.0731(2) -0.0454(9) -0.0745(4) 0.065(3) Uij ? ? O(10) 0.0718(3) -0.039(1) -0.1738(4) 0.087(4) Uij ? ? O(11) 0.1521(2) 0.0171(8) 0.1133(4) 0.055(3) Uij ? ? O(12) 0.1115(3) 0.1342(8) 0.1051(4) 0.064(3) Uij ? ? O(13) 0.1366(3) 0.108(1) 0.1925(4) 0.087(4) Uij ? ? O(14) 0.0813(3) 0.1919(10) -0.0214(5) 0.085(4) Uij ? ? O(15) 0.1733(2) -0.2024(8) 0.0863(4) 0.059(3) Uij ? ? O(16) 0.1803(2) -0.3444(9) 0.0292(4) 0.064(3) Uij ? ? O(17) 0.2237(3) -0.2599(9) 0.0709(5) 0.077(4) Uij ? ? O(18) 0.1303 -0.4433 -0.0440 0.0774 Uij ? ? O(19) 0.0935 -0.4956 0.0071 0.1467 Uij ? ? O(20) 0.1158 -0.5988 -0.0693 0.1814 Uij ? ? O(21) 0.0730 -0.4687 0.0475 0.0890 Uij ? ? O(22) 0.0576 -0.3382 0.0964 0.0762 Uij ? ? O(23) 0.0288 -0.4674 0.0858 0.2088 Uij ? ? O(24) 0.0676(3) -0.2686(9) -0.0411(5) 0.076(4) Uij ? ? O(25) 0.1372(3) -0.4409(9) 0.1220(5) 0.074(4) Uij ? ? O(26) 0.2136(4) 0.487(1) -0.2892(8) 0.176(8) Uij ? ? O(27) 0.2302(3) 0.336(1) -0.2489(7) 0.121(6) Uij ? ? O(28) 0.1848(3) 0.3454(10) -0.3028(6) 0.097(5) Uij ? ? O(29) 0.2135(3) 0.1986(10) 0.1164(5) 0.092(5) Uij ? ? O(30) 0.0570(7) 0.260(2) 0.214(1) 0.34(2) Uij ? ? N(1) 0.2293(2) -0.0243(10) 0.1132(5) 0.048(3) Uij ? ? N(2) 0.2348(3) -0.0610(10) -0.0303(5) 0.055(4) Uij ? ? N(3) 0.1814(3) -0.1156(10) 0.2179(4) 0.050(3) Uij ? ? N(4) 0.1062(3) -0.129(1) 0.2398(5) 0.056(4) Uij ? ? N(5) 0.1708(4) 0.239(1) -0.0285(7) 0.077(5) Uij ? ? N(6) 0.0859(3) -0.016(1) -0.1246(5) 0.059(4) Uij ? ? N(7) 0.1331(3) 0.086(1) 0.1381(5) 0.057(4) Uij ? ? N(8) 0.1925(3) -0.269(1) 0.0625(5) 0.056(4) Uij ? ? N(9) 0.1151 -0.4985 -0.0372 0.1080 Uij ? ? N(10) 0.0561 -0.4123 0.0835 0.1127 Uij ? ? N(11) 0.2107(4) 0.387(1) -0.2785(7) 0.082(4) Uij ? ? C(1) 0.2375(3) -0.073(1) 0.1746(6) 0.062(5) Uij ? ? C(2) 0.2598(3) -0.024(1) 0.0745(7) 0.065(5) Uij ? ? C(3) 0.2529(3) 0.016(1) 0.0096(7) 0.060(5) Uij ? ? C(4) 0.2020(3) -0.060(1) -0.0382(6) 0.044(4) Uij ? ? C(5) 0.1873(3) -0.129(1) -0.0872(5) 0.042(4) Uij ? ? C(6) 0.1553(3) -0.172(1) -0.0811(6) 0.048(4) Uij ? ? C(7) 0.1419(4) -0.237(1) -0.1323(6) 0.065(5) Uij ? ? C(8) 0.1598(5) -0.258(1) -0.1828(6) 0.070(6) Uij ? ? C(9) 0.1914(4) -0.217(1) -0.1881(6) 0.065(5) Uij ? ? C(10) 0.2050(3) -0.155(1) -0.1399(6) 0.055(5) Uij ? ? C(11) 0.2126(4) -0.046(1) 0.2224(6) 0.062(5) Uij ? ? C(12) 0.1646(4) -0.118(1) 0.2782(6) 0.059(5) Uij ? ? C(13) 0.1332(4) -0.186(1) 0.2735(6) 0.057(5) Uij ? ? C(14) 0.0983(3) -0.157(1) 0.1829(6) 0.052(4) Uij ? ? C(15) 0.0683(3) -0.101(1) 0.1530(6) 0.051(4) Uij ? ? C(16) 0.0666(3) -0.078(1) 0.0903(5) 0.043(4) Uij ? ? C(17) 0.0390(3) -0.024(2) 0.0657(6) 0.070(5) Uij ? ? C(18) 0.0136(4) 0.008(2) 0.1012(7) 0.123(8) Uij ? ? C(19) 0.0147(4) -0.015(2) 0.1632(7) 0.097(7) Uij ? ? C(20) 0.0419(4) -0.070(2) 0.1894(6) 0.075(6) Uij ? ? C(21) 0.1437(6) -0.556(2) 0.1149(10) 0.14(1) Uij ? ? C(22) 0.2351(5) 0.290(2) 0.1293(10) 0.104(8) Uij ? ? H(1) 0.2586 -0.0463 0.1885 0.0741 Uij ? ? H(2) 0.2385 -0.1515 0.1702 0.0741 Uij ? ? H(3) 0.2761 0.0223 0.0937 0.0780 Uij ? ? H(4) 0.2681 -0.0979 0.0727 0.0780 Uij ? ? H(5) 0.2737 0.0314 -0.0083 0.0720 Uij ? ? H(6) 0.2403 0.0825 0.0117 0.0720 Uij ? ? H(7) 0.1199 -0.2651 -0.1306 0.0778 Uij ? ? H(8) 0.1503 -0.3025 -0.2150 0.0844 Uij ? ? H(9) 0.2036 -0.2301 -0.2240 0.0780 Uij ? ? H(10) 0.2272 -0.1286 -0.1426 0.0664 Uij ? ? H(11) 0.2229 -0.0577 0.2620 0.0748 Uij ? ? H(12) 0.2065 0.0292 0.2180 0.0748 Uij ? ? H(13) 0.1793 -0.1495 0.3086 0.0708 Uij ? ? H(14) 0.1592 -0.0443 0.2898 0.0708 Uij ? ? H(15) 0.1262 -0.2013 0.3140 0.0684 Uij ? ? H(16) 0.2081 0.0031 0.1001 0.0575 Uij ? ? H(17) 0.2470 -0.1151 -0.0518 0.0662 Uij ? ? H(18) 0.1734 -0.1526 0.1816 0.0605 Uij ? ? H(19) 0.0942 -0.0723 0.2593 0.0666 Uij ? ? H(20) 0.1379 -0.2531 0.2529 0.0684 Uij ? ? H(21) 0.0377 -0.0091 0.0227 0.0845 Uij ? ? H(22) -0.0050 0.0463 0.0832 0.1482 Uij ? ? H(23) -0.0031 0.0065 0.1881 0.1163 Uij ? ? H(24) 0.0427 -0.0862 0.2323 0.0894 Uij ? ? H(25) 0.1235 -0.5935 0.1034 0.1632 Uij ? ? H(26) 0.1594 -0.5667 0.0838 0.1632 Uij ? ? H(27) 0.1523 -0.5857 0.1528 0.1632 Uij ? ? 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 La(1) 0.0358(4) 0.0532(5) 0.0360(4) 0.0031(4) 0.0025(3) -0.0039(4) La(2) 0.0461(5) 0.0562(6) 0.0416(4) -0.0020(5) 0.0024(3) -0.0044(4) O(1) 0.037(5) 0.058(7) 0.073(6) 0.006(5) 0.009(5) -0.023(5) O(2) 0.044(5) 0.059(6) 0.034(4) -0.001(5) 0.012(4) -0.007(4) O(3) 0.063(7) 0.074(8) 0.039(5) 0.018(6) 0.001(5) -0.005(5) O(4) 0.037(5) 0.067(7) 0.037(5) 0.000(5) 0.007(4) 0.005(5) O(5) 0.077(8) 0.11(1) 0.056(6) -0.039(7) -0.008(6) 0.011(7) O(6) 0.063(7) 0.068(8) 0.064(7) -0.003(6) -0.004(5) -0.007(6) O(7) 0.18(2) 0.14(1) 0.13(1) -0.12(1) 0.02(1) -0.01(1) O(8) 0.046(6) 0.070(7) 0.053(5) -0.018(6) 0.002(4) 0.007(5) O(9) 0.041(5) 0.109(9) 0.047(5) -0.004(6) 0.005(4) 0.011(6) O(10) 0.075(8) 0.14(1) 0.047(6) -0.023(8) -0.020(5) 0.006(7) O(11) 0.051(6) 0.060(7) 0.054(6) 0.011(5) -0.008(5) -0.013(5) O(12) 0.076(8) 0.069(7) 0.047(6) 0.022(6) 0.007(5) -0.011(5) O(13) 0.103(9) 0.11(1) 0.046(6) 0.027(8) -0.012(6) -0.025(7) O(14) 0.087(9) 0.082(9) 0.086(8) 0.015(7) -0.015(6) 0.007(7) O(15) 0.053(6) 0.068(7) 0.055(6) 0.021(6) -0.004(5) -0.025(5) O(16) 0.061(7) 0.065(7) 0.066(6) 0.006(6) 0.005(5) -0.021(6) O(17) 0.050(7) 0.071(8) 0.109(9) -0.001(6) 0.004(6) -0.019(7) O(24) 0.071(8) 0.088(9) 0.069(7) -0.013(7) -0.008(6) 0.009(6) O(25) 0.092(9) 0.051(7) 0.079(7) 0.014(6) -0.004(6) 0.005(6) O(26) 0.20(2) 0.11(1) 0.21(2) -0.07(1) -0.15(1) 0.06(1) O(27) 0.11(1) 0.10(1) 0.15(1) -0.005(9) -0.066(10) 0.036(9) O(28) 0.095(10) 0.082(9) 0.112(10) -0.028(8) -0.040(8) 0.017(8) O(29) 0.103(10) 0.074(9) 0.099(9) 0.016(8) -0.013(7) -0.017(7) O(30) 0.35(4) 0.31(4) 0.35(4) 0.04(3) 0.08(3) 0.15(3) N(1) 0.027(6) 0.066(8) 0.050(6) 0.007(6) 0.004(5) -0.002(6) N(2) 0.039(7) 0.065(9) 0.063(7) -0.004(6) 0.010(5) -0.012(6) N(3) 0.044(7) 0.072(8) 0.035(6) 0.000(6) -0.004(5) -0.007(6) N(4) 0.047(7) 0.085(9) 0.035(6) 0.020(7) 0.002(5) -0.008(6) N(5) 0.09(1) 0.08(1) 0.065(9) -0.015(9) 0.001(8) -0.003(8) N(6) 0.058(8) 0.08(1) 0.037(6) 0.007(8) 0.003(6) 0.005(7) N(7) 0.060(8) 0.067(9) 0.043(7) 0.005(7) -0.008(6) -0.012(6) N(8) 0.060(9) 0.055(9) 0.052(7) 0.004(7) -0.002(6) -0.002(6) C(1) 0.041(8) 0.09(1) 0.053(8) -0.002(8) -0.001(7) -0.008(8) C(2) 0.034(8) 0.08(1) 0.08(1) -0.015(8) 0.000(7) -0.010(10) C(3) 0.039(8) 0.07(1) 0.070(10) -0.004(8) 0.009(7) -0.013(9) C(4) 0.037(8) 0.045(9) 0.052(8) 0.003(7) 0.008(6) 0.005(7) C(5) 0.038(8) 0.056(9) 0.034(6) 0.003(7) 0.007(5) -0.005(6) C(6) 0.041(8) 0.053(10) 0.050(8) 0.008(7) -0.006(6) -0.007(7) C(7) 0.052(9) 0.09(1) 0.047(8) 0.004(9) -0.004(7) -0.014(8) C(8) 0.09(1) 0.08(1) 0.037(8) -0.01(1) 0.005(8) -0.008(8) C(9) 0.07(1) 0.08(1) 0.041(8) 0.00(1) 0.010(7) -0.009(8) C(10) 0.051(9) 0.07(1) 0.047(8) 0.013(8) 0.012(7) 0.007(8) C(11) 0.058(9) 0.08(1) 0.050(8) -0.008(9) -0.007(7) -0.023(9) C(12) 0.049(9) 0.09(1) 0.041(7) 0.007(9) -0.006(6) -0.009(8) C(13) 0.07(1) 0.07(1) 0.031(7) 0.010(9) 0.007(7) 0.002(7) C(14) 0.054(9) 0.07(1) 0.036(7) 0.004(8) 0.006(6) 0.008(7) C(15) 0.031(7) 0.08(1) 0.042(7) 0.004(7) 0.007(6) -0.001(7) C(16) 0.033(7) 0.067(10) 0.031(6) 0.005(7) 0.006(5) 0.003(6) C(17) 0.042(8) 0.13(2) 0.036(7) 0.02(1) 0.001(6) 0.004(9) C(18) 0.043(9) 0.28(3) 0.051(9) 0.07(1) -0.003(7) -0.01(1) C(19) 0.038(9) 0.19(2) 0.059(10) 0.02(1) 0.012(7) -0.02(1) C(20) 0.047(9) 0.14(2) 0.036(7) 0.02(1) 0.010(6) -0.011(9) C(21) 0.14(2) 0.16(2) 0.11(2) -0.01(2) -0.05(2) -0.01(2) C(22) 0.12(2) 0.07(1) 0.13(2) -0.03(1) -0.02(1) -0.01(1) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 6803 _refine_ls_number_parameters 509 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0660 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0863 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.857 _refine_ls_shift/esd_max 0.0340 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.69 _refine_diff_density_max 1.52 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag La(1) O(1) 2.472(9) ? ? yes La(1) O(2) 2.473(9) ? ? yes La(1) O(4) 2.464(8) ? ? yes La(1) O(5) 2.71(1) ? ? yes La(1) O(6) 2.70(1) ? ? yes La(1) O(8) 2.654(8) ? ? yes La(1) O(9) 2.748(9) ? ? yes La(1) O(11) 2.690(9) ? ? yes La(1) O(12) 2.669(9) ? ? yes La(1) O(14) 2.60(1) ? ? yes La(2) O(2) 2.520(8) ? ? yes La(2) O(3) 2.498(9) ? ? yes La(2) O(4) 2.460(9) ? ? yes La(2) O(15) 2.728(9) ? ? yes La(2) O(16) 2.740(10) ? ? yes La(2) O(18) 2.7285(8) ? ? yes La(2) O(19) 2.6970(9) ? ? yes La(2) O(21) 2.6961(9) ? ? yes La(2) O(22) 2.6372(8) ? ? yes La(2) O(24) 2.623(10) ? ? yes La(2) O(25) 2.59(1) ? ? yes La(2) N(10) 2.9001(8) ? ? yes O(1) C(4) 1.23(1) ? ? yes O(2) C(6) 1.34(1) ? ? yes O(3) C(14) 1.27(2) ? ? yes O(4) C(16) 1.37(1) ? ? yes O(5) N(5) 1.27(2) ? ? yes O(6) N(5) 1.25(2) ? ? yes O(7) N(5) 1.22(2) ? ? yes O(8) N(6) 1.24(1) ? ? yes O(9) N(6) 1.27(1) ? ? yes O(10) N(6) 1.22(1) ? ? yes O(11) N(7) 1.26(1) ? ? yes O(12) N(7) 1.25(1) ? ? yes O(13) N(7) 1.21(1) ? ? yes O(15) N(8) 1.24(1) ? ? yes O(16) N(8) 1.25(1) ? ? yes O(17) N(8) 1.26(1) ? ? yes O(18) N(9) 0.919 ? ? yes O(19) O(21) 1.265 ? ? yes O(19) N(9) 1.319 ? ? yes O(20) N(9) 1.397 ? ? yes O(21) N(10) 1.253 ? ? yes O(22) N(10) 0.938 ? ? yes O(23) N(10) 1.285 ? ? yes O(25) C(21) 1.43(3) ? ? yes O(26) N(11) 1.25(2) ? ? yes O(27) N(11) 1.17(2) ? ? yes O(28) N(11) 1.25(2) ? ? yes O(29) C(22) 1.43(2) ? ? yes N(1) C(1) 1.48(2) ? ? yes N(1) C(2) 1.51(2) ? ? yes N(2) C(3) 1.45(2) ? ? yes N(2) C(4) 1.32(2) ? ? yes N(3) C(11) 1.51(2) ? ? yes N(3) C(12) 1.49(2) ? ? yes N(4) C(13) 1.46(2) ? ? yes N(4) C(14) 1.31(2) ? ? yes C(1) C(11) 1.50(2) ? ? yes C(2) C(3) 1.51(2) ? ? yes C(4) C(5) 1.46(2) ? ? yes C(5) C(6) 1.40(2) ? ? yes C(5) C(10) 1.40(2) ? ? yes C(6) C(7) 1.44(2) ? ? yes C(7) C(8) 1.35(2) ? ? yes C(8) C(9) 1.37(2) ? ? yes C(9) C(10) 1.38(2) ? ? yes C(12) C(13) 1.50(2) ? ? yes C(14) C(15) 1.50(2) ? ? yes C(15) C(16) 1.39(2) ? ? yes C(15) C(20) 1.40(2) ? ? yes C(16) C(17) 1.38(2) ? ? yes C(17) C(18) 1.36(2) ? ? yes C(18) C(19) 1.37(2) ? ? yes C(19) C(20) 1.38(2) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) La(1) O(2) 68.3(3) ? ? ? yes O(1) La(1) O(4) 115.4(3) ? ? ? yes O(1) La(1) O(5) 68.2(3) ? ? ? yes O(1) La(1) O(6) 67.6(3) ? ? ? yes O(1) La(1) O(8) 96.3(3) ? ? ? yes O(1) La(1) O(9) 130.1(3) ? ? ? yes O(1) La(1) O(11) 69.1(3) ? ? ? yes O(1) La(1) O(12) 109.3(3) ? ? ? yes O(1) La(1) O(14) 141.2(3) ? ? ? yes O(2) La(1) O(4) 66.0(3) ? ? ? yes O(2) La(1) O(5) 112.6(3) ? ? ? yes O(2) La(1) O(6) 135.9(3) ? ? ? yes O(2) La(1) O(8) 75.4(3) ? ? ? yes O(2) La(1) O(9) 69.8(3) ? ? ? yes O(2) La(1) O(11) 95.7(3) ? ? ? yes O(2) La(1) O(12) 134.5(3) ? ? ? yes O(2) La(1) O(14) 140.5(3) ? ? ? yes O(4) La(1) O(5) 173.9(3) ? ? ? yes O(4) La(1) O(6) 138.9(3) ? ? ? yes O(4) La(1) O(8) 112.9(3) ? ? ? yes O(4) La(1) O(9) 68.5(3) ? ? ? yes O(4) La(1) O(11) 72.7(3) ? ? ? yes O(4) La(1) O(12) 76.4(3) ? ? ? yes O(4) La(1) O(14) 102.4(3) ? ? ? yes O(5) La(1) O(6) 46.5(3) ? ? ? yes O(5) La(1) O(8) 61.3(3) ? ? ? yes O(5) La(1) O(9) 105.4(3) ? ? ? yes O(5) La(1) O(11) 113.4(3) ? ? ? yes O(5) La(1) O(12) 107.4(3) ? ? ? yes O(5) La(1) O(14) 74.8(4) ? ? ? yes O(6) La(1) O(8) 107.2(3) ? ? ? yes O(6) La(1) O(9) 143.8(3) ? ? ? yes O(6) La(1) O(11) 70.8(3) ? ? ? yes O(6) La(1) O(12) 65.2(3) ? ? ? yes O(6) La(1) O(14) 78.6(3) ? ? ? yes O(8) La(1) O(9) 47.1(3) ? ? ? yes O(8) La(1) O(11) 165.1(3) ? ? ? yes O(8) La(1) O(12) 145.9(3) ? ? ? yes O(8) La(1) O(14) 75.5(3) ? ? ? yes O(9) La(1) O(11) 141.2(3) ? ? ? yes O(9) La(1) O(12) 119.2(3) ? ? ? yes O(9) La(1) O(14) 70.8(3) ? ? ? yes O(11) La(1) O(12) 47.5(3) ? ? ? yes O(11) La(1) O(14) 117.6(3) ? ? ? yes O(12) La(1) O(14) 70.5(3) ? ? ? yes O(2) La(2) O(3) 115.6(3) ? ? ? yes O(2) La(2) O(4) 65.3(3) ? ? ? yes O(2) La(2) O(15) 68.9(3) ? ? ? yes O(2) La(2) O(16) 72.9(3) ? ? ? yes O(2) La(2) O(18) 82.5(2) ? ? ? yes O(2) La(2) O(19) 120.1(2) ? ? ? yes O(2) La(2) O(21) 139.0(2) ? ? ? yes O(2) La(2) O(22) 137.8(2) ? ? ? yes O(2) La(2) O(24) 73.3(3) ? ? ? yes O(2) La(2) O(25) 139.0(3) ? ? ? yes O(2) La(2) N(10) 144.8(2) ? ? ? yes O(3) La(2) O(4) 67.9(3) ? ? ? yes O(3) La(2) O(15) 65.2(3) ? ? ? yes O(3) La(2) O(16) 102.3(3) ? ? ? yes O(3) La(2) O(18) 152.1(2) ? ? ? yes O(3) La(2) O(19) 124.3(2) ? ? ? yes O(3) La(2) O(21) 102.1(2) ? ? ? yes O(3) La(2) O(22) 68.8(2) ? ? ? yes O(3) La(2) O(24) 128.2(3) ? ? ? yes O(3) La(2) O(25) 67.1(3) ? ? ? yes O(3) La(2) N(10) 81.9(2) ? ? ? yes O(4) La(2) O(15) 84.9(3) ? ? ? yes O(4) La(2) O(16) 124.8(3) ? ? ? yes O(4) La(2) O(18) 139.6(2) ? ? ? yes O(4) La(2) O(19) 138.6(2) ? ? ? yes O(4) La(2) O(21) 119.9(2) ? ? ? yes O(4) La(2) O(22) 80.4(2) ? ? ? yes O(4) La(2) O(24) 72.1(3) ? ? ? yes O(4) La(2) O(25) 135.0(3) ? ? ? yes O(4) La(2) N(10) 97.8(2) ? ? ? yes O(15) La(2) O(16) 46.1(3) ? ? ? yes O(15) La(2) O(18) 106.4(2) ? ? ? yes O(15) La(2) O(19) 136.4(2) ? ? ? yes O(15) La(2) O(21) 147.0(2) ? ? ? yes O(15) La(2) O(22) 134.0(2) ? ? ? yes O(15) La(2) O(24) 141.3(3) ? ? ? yes O(15) La(2) O(25) 77.5(3) ? ? ? yes O(15) La(2) N(10) 143.4(2) ? ? ? yes O(16) La(2) O(18) 61.2(2) ? ? ? yes O(16) La(2) O(19) 93.1(2) ? ? ? yes O(16) La(2) O(21) 115.3(2) ? ? ? yes O(16) La(2) O(22) 149.3(2) ? ? ? yes O(16) La(2) O(24) 127.7(3) ? ? ? yes O(16) La(2) O(25) 66.9(3) ? ? ? yes O(16) La(2) N(10) 135.9(2) ? ? ? yes O(18) La(2) O(19) 42.83(1) ? ? ? yes O(18) La(2) O(21) 69.86(2) ? ? ? yes O(18) La(2) O(22) 112.95(3) ? ? ? yes O(18) La(2) O(24) 75.8(2) ? ? ? yes O(18) La(2) O(25) 85.3(2) ? ? ? yes O(18) La(2) N(10) 95.00(3) ? ? ? yes O(19) La(2) O(21) 27.132(9) ? ? ? yes O(19) La(2) O(22) 71.12(2) ? ? ? yes O(19) La(2) O(24) 71.3(2) ? ? ? yes O(19) La(2) O(25) 71.0(2) ? ? ? yes O(19) La(2) N(10) 52.60(2) ? ? ? yes O(21) La(2) O(22) 44.22(1) ? ? ? yes O(21) La(2) O(24) 71.0(2) ? ? ? yes O(21) La(2) O(25) 69.6(3) ? ? ? yes O(21) La(2) N(10) 25.546(8) ? ? ? yes O(22) La(2) O(24) 73.2(2) ? ? ? yes O(22) La(2) O(25) 82.8(3) ? ? ? yes O(22) La(2) N(10) 18.747(6) ? ? ? yes O(24) La(2) O(25) 140.1(3) ? ? ? yes O(24) La(2) N(10) 72.1(2) ? ? ? yes O(25) La(2) N(10) 75.1(3) ? ? ? yes La(1) O(1) C(4) 132.5(9) ? ? ? yes La(1) O(2) La(2) 111.2(3) ? ? ? yes La(1) O(2) C(6) 117.2(8) ? ? ? yes La(2) O(2) C(6) 131.3(8) ? ? ? yes La(2) O(3) C(14) 134.0(8) ? ? ? yes La(1) O(4) La(2) 113.5(3) ? ? ? yes La(1) O(4) C(16) 123.0(8) ? ? ? yes La(2) O(4) C(16) 123.1(8) ? ? ? yes La(1) O(5) N(5) 97.4(9) ? ? ? yes La(1) O(6) N(5) 98.8(9) ? ? ? yes La(1) O(8) N(6) 99.8(7) ? ? ? yes La(1) O(9) N(6) 94.4(8) ? ? ? yes La(1) O(11) N(7) 96.3(7) ? ? ? yes La(1) O(12) N(7) 97.6(7) ? ? ? yes La(2) O(15) N(8) 98.2(8) ? ? ? yes La(2) O(16) N(8) 97.1(8) ? ? ? yes La(2) O(18) N(9) 101.36(2) ? ? ? yes La(2) O(19) O(21) 76.39(2) ? ? ? yes La(2) O(19) N(9) 92.12(2) ? ? ? yes O(21) O(19) N(9) 166.6486(2) ? ? ? yes La(2) O(21) O(19) 76.48(2) ? ? ? yes La(2) O(21) N(10) 86.36(2) ? ? ? yes O(19) O(21) N(10) 161.7768(1) ? ? ? yes La(2) O(22) N(10) 96.67(2) ? ? ? yes La(2) O(25) C(21) 131(1) ? ? ? yes C(1) N(1) C(2) 110(1) ? ? ? yes C(3) N(2) C(4) 123(1) ? ? ? yes C(11) N(3) C(12) 110(1) ? ? ? yes C(13) N(4) C(14) 120(1) ? ? ? yes O(5) N(5) O(6) 115(1) ? ? ? yes O(5) N(5) O(7) 123(1) ? ? ? yes O(6) N(5) O(7) 120(1) ? ? ? yes O(8) N(6) O(9) 118(1) ? ? ? yes O(8) N(6) O(10) 121(1) ? ? ? yes O(9) N(6) O(10) 119(1) ? ? ? yes O(11) N(7) O(12) 118(1) ? ? ? yes O(11) N(7) O(13) 120(1) ? ? ? yes O(12) N(7) O(13) 120(1) ? ? ? yes O(15) N(8) O(16) 118(1) ? ? ? yes O(15) N(8) O(17) 120(1) ? ? ? yes O(16) N(8) O(17) 120(1) ? ? ? yes O(18) N(9) O(19) 123.6597(7) ? ? ? yes O(18) N(9) O(20) 121.7141(5) ? ? ? yes O(19) N(9) O(20) 114.2373(2) ? ? ? yes La(2) N(10) O(21) 68.09(2) ? ? ? yes La(2) N(10) O(22) 64.58(2) ? ? ? yes La(2) N(10) O(23) 165.40(2) ? ? ? yes O(21) N(10) O(22) 132.2809(5) ? ? ? yes O(21) N(10) O(23) 102.896(1) ? ? ? yes O(22) N(10) O(23) 121.9190(5) ? ? ? yes O(26) N(11) O(27) 123(1) ? ? ? yes O(26) N(11) O(28) 113(1) ? ? ? yes O(27) N(11) O(28) 123(1) ? ? ? yes N(1) C(1) C(11) 113(1) ? ? ? yes N(1) C(2) C(3) 113(1) ? ? ? yes N(2) C(3) C(2) 114(1) ? ? ? yes O(1) C(4) N(2) 119(1) ? ? ? yes O(1) C(4) C(5) 123(1) ? ? ? yes N(2) C(4) C(5) 117(1) ? ? ? yes C(4) C(5) C(6) 119(1) ? ? ? yes C(4) C(5) C(10) 121(1) ? ? ? yes C(6) C(5) C(10) 119(1) ? ? ? yes O(2) C(6) C(5) 125(1) ? ? ? yes O(2) C(6) C(7) 118(1) ? ? ? yes C(5) C(6) C(7) 116(1) ? ? ? yes C(6) C(7) C(8) 122(1) ? ? ? yes C(7) C(8) C(9) 121(1) ? ? ? yes C(8) C(9) C(10) 118(1) ? ? ? yes C(5) C(10) C(9) 122(1) ? ? ? yes N(3) C(11) C(1) 114(1) ? ? ? yes N(3) C(12) C(13) 110(1) ? ? ? yes N(4) C(13) C(12) 112(1) ? ? ? yes O(3) C(14) N(4) 121(1) ? ? ? yes O(3) C(14) C(15) 121(1) ? ? ? yes N(4) C(14) C(15) 117(1) ? ? ? yes C(14) C(15) C(16) 121(1) ? ? ? yes C(14) C(15) C(20) 119(1) ? ? ? yes C(16) C(15) C(20) 119(1) ? ? ? yes O(4) C(16) C(15) 120(1) ? ? ? yes O(4) C(16) C(17) 119(1) ? ? ? yes C(15) C(16) C(17) 119(1) ? ? ? yes C(16) C(17) C(18) 121(1) ? ? ? yes C(17) C(18) C(19) 119(1) ? ? ? yes C(18) C(19) C(20) 120(1) ? ? ? yes C(15) C(20) C(19) 120(1) ? ? ? yes #------------------------------------------------------------------------------ #============END OF FILE=========================== data_wtwong810-winnie013-complex_2 _database_code_CSD 175402 #------------------------------------------------------------------------------ _audit_creation_date 'Sat Sep 25 17:46:24 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 22.760(1) _cell_length_b 10.847(1) _cell_length_c 21.550(1) _cell_angle_alpha 90 _cell_angle_beta 106.83(2) _cell_angle_gamma 90 _cell_volume 5092.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c' 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' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.240 _exptl_crystal_size_min 0.220 _exptl_crystal_density_diffrn 1.709 _exptl_crystal_density_meas ? _chemical_formula_weight 1310.58 _chemical_formula_analytical ? _chemical_formula_sum 'C28 H48 N14 O28 Pr2 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2624.00 _exptl_absorpt_coefficient_mu 1.984 _exptl_absorpt_correction_type inter-image scaling #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'Marresearch Imaging Plate System' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 17167 _reflns_number_total 4639 _reflns_number_observed 3342 _reflns_observed_criterion 1.50 _diffrn_reflns_av_R_equivalents 0.03 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.56 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pr 0 8 -0.218 2.821 'International Tables' C 0 112 0.003 0.002 'International Tables' N 0 56 0.006 0.003 'International Tables' O 0 112 0.011 0.006 'International Tables' H 0 192 0.000 0.000 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Pr(1) 0.07868(1) -0.00323(3) 0.22876(1) 0.0357(1) Uij ? ? O(1) -0.0320(2) 0.1362(4) 0.3609(2) 0.048(1) Uij ? ? O(2) 0.0310(2) -0.0412(4) 0.3121(2) 0.038(1) Uij ? ? O(3) 0.0652(2) 0.2144(4) 0.2758(2) 0.052(1) Uij ? ? O(4) 0.1470(2) 0.1159(4) 0.3272(2) 0.053(1) Uij ? ? O(5) 0.1308(2) 0.3013(5) 0.3567(3) 0.079(2) Uij ? ? O(6) 0.0653(2) -0.2408(4) 0.2103(2) 0.055(1) Uij ? ? O(7) 0.0829(2) -0.1331(4) 0.1327(2) 0.055(1) Uij ? ? O(8) 0.0632(3) -0.3293(5) 0.1182(3) 0.086(2) Uij ? ? O(9) 0.1749(2) -0.1131(4) 0.2824(2) 0.062(1) Uij ? ? O(10) 0.1587(2) 0.1153(4) 0.1916(2) 0.063(1) Uij ? ? O(11) 0.6494(3) 0.1443(6) 0.6346(3) 0.106(2) Uij ? ? O(12) 0.7095(3) 0.0017(4) 0.6835(3) 0.077(2) Uij ? ? O(13) 0.6323(3) 0.0494(7) 0.7157(3) 0.093(2) Uij ? ? O(14) 0.2134(2) -0.3545(5) 0.2990(2) 0.075(1) Uij ? ? N(1) -0.0027(2) 0.4085(4) 0.3252(2) 0.048(2) Uij ? ? N(2) 0.0397(3) 0.2248(5) 0.4451(2) 0.054(2) Uij ? ? N(3) 0.1149(2) 0.2128(5) 0.3205(2) 0.049(2) Uij ? ? N(4) 0.0700(2) -0.2368(5) 0.1526(3) 0.058(2) Uij ? ? N(5) 0.6632(3) 0.0662(6) 0.6775(3) 0.064(2) Uij ? ? N(6) 0.3317(5) 0.2466(10) 0.4663(5) 0.142(4) Uij ? ? N(7) 0.2827(4) 0.0699(9) 0.0760(5) 0.122(3) Uij ? ? C(1) 0.0177(3) 0.5034(5) 0.2855(4) 0.053(2) Uij ? ? C(2) 0.0254(3) 0.4348(6) 0.3972(3) 0.060(2) Uij ? ? C(3) 0.0069(3) 0.3417(7) 0.4409(3) 0.059(2) Uij ? ? C(4) 0.0169(3) 0.1270(6) 0.4081(3) 0.045(2) Uij ? ? C(5) 0.0508(3) 0.0089(5) 0.4250(3) 0.039(2) Uij ? ? C(6) 0.0553(2) -0.0713(5) 0.3755(3) 0.038(2) Uij ? ? C(7) 0.0841(3) -0.1830(6) 0.3920(3) 0.050(2) Uij ? ? C(8) 0.1073(4) -0.2171(6) 0.4567(4) 0.066(2) Uij ? ? C(9) 0.1038(3) -0.1375(7) 0.5050(3) 0.063(2) Uij ? ? C(10) 0.0758(3) -0.0247(6) 0.4888(3) 0.050(2) Uij ? ? C(11) 0.2727(5) 0.3068(9) 0.3552(5) 0.098(3) Uij ? ? C(12) 0.3032(5) 0.2780(9) 0.4175(5) 0.090(3) Uij ? ? C(13) 0.2406(7) 0.0160(10) -0.0451(7) 0.123(4) Uij ? ? C(14) 0.2635(5) 0.049(1) 0.0230(5) 0.101(3) Uij ? ? H(1) 0.0597 0.4900 0.2895 0.0623 Uij ? ? H(2) 0.0126 0.5817 0.3030 0.0623 Uij ? ? H(3) 0.0685 0.4353 0.4068 0.0726 Uij ? ? H(4) 0.0114 0.5141 0.4058 0.0726 Uij ? ? H(5) 0.0155 0.3755 0.4831 0.0711 Uij ? ? H(6) -0.0358 0.3258 0.4242 0.0711 Uij ? ? H(7) 0.0880 -0.2372 0.3590 0.0607 Uij ? ? H(8) 0.1259 -0.2955 0.4676 0.0792 Uij ? ? H(9) 0.1202 -0.1610 0.5490 0.0752 Uij ? ? H(10) 0.0733 0.0298 0.5222 0.0597 Uij ? ? H(11) 0.0095 0.3377 0.3165 0.0570 Uij ? ? H(12) 0.0737 0.2188 0.4715 0.0650 Uij ? ? H(13) 0.2157 -0.0738 0.3018 0.0585 Uij ? ? H(14) 0.1831 -0.1889 0.2891 0.0585 Uij ? ? H(15) 0.1366 0.1624 0.1578 0.0585 Uij ? ? H(16) 0.2015 0.1139 0.2127 0.0585 Uij ? ? H(17) 0.2406 0.3640 0.3550 0.1194 Uij ? ? H(18) 0.3002 0.3442 0.3353 0.1194 Uij ? ? H(19) 0.2559 0.2347 0.3331 0.1194 Uij ? ? H(20) 0.2111 0.0742 -0.0664 0.1451 Uij ? ? H(21) 0.2736 0.0137 -0.0636 0.1451 Uij ? ? H(22) 0.2221 -0.0641 -0.0486 0.1451 Uij ? ? 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 Pr(1) 0.0314(2) 0.0352(2) 0.0404(2) -0.0010(1) 0.0104(1) -0.0012(1) O(1) 0.046(3) 0.047(2) 0.047(2) 0.009(2) 0.009(2) -0.009(2) O(2) 0.036(2) 0.040(2) 0.038(2) 0.006(2) 0.009(2) 0.000(2) O(3) 0.040(2) 0.044(2) 0.068(3) 0.003(2) 0.011(2) -0.005(2) O(4) 0.043(3) 0.048(3) 0.063(3) 0.009(2) 0.006(2) -0.010(2) O(5) 0.056(3) 0.071(4) 0.105(4) -0.006(3) 0.018(3) -0.047(3) O(6) 0.066(3) 0.046(3) 0.058(3) -0.009(2) 0.025(2) -0.005(2) O(7) 0.062(3) 0.045(3) 0.062(3) -0.007(2) 0.025(2) -0.004(2) O(8) 0.102(5) 0.067(4) 0.095(4) -0.023(3) 0.037(3) -0.037(3) O(9) 0.045(3) 0.041(3) 0.091(3) 0.011(2) 0.005(2) -0.002(2) O(10) 0.044(3) 0.068(3) 0.074(3) -0.013(2) 0.013(2) 0.008(2) O(11) 0.122(6) 0.078(4) 0.120(5) 0.038(4) 0.039(4) 0.034(4) O(12) 0.056(3) 0.064(3) 0.116(5) 0.017(3) 0.032(3) 0.011(3) O(13) 0.058(4) 0.136(5) 0.093(5) 0.009(4) 0.035(3) 0.004(4) N(1) 0.051(3) 0.032(3) 0.064(3) 0.003(2) 0.021(3) -0.003(2) N(2) 0.059(4) 0.047(3) 0.050(3) 0.007(3) 0.003(3) -0.006(2) N(3) 0.040(3) 0.054(3) 0.054(3) -0.004(3) 0.014(2) -0.017(3) N(4) 0.046(3) 0.046(3) 0.081(4) -0.002(3) 0.016(3) -0.020(3) N(5) 0.061(4) 0.048(4) 0.082(4) -0.003(3) 0.018(4) 0.003(3) C(1) 0.057(4) 0.033(3) 0.081(5) -0.005(3) 0.040(4) -0.012(3) C(2) 0.059(4) 0.045(4) 0.074(5) -0.001(3) 0.018(4) -0.022(3) C(3) 0.068(5) 0.059(4) 0.051(4) 0.012(4) 0.018(3) -0.015(3) C(4) 0.047(4) 0.046(4) 0.042(3) 0.000(3) 0.016(3) 0.001(3) C(5) 0.036(3) 0.044(3) 0.038(3) 0.006(3) 0.011(2) 0.005(2) C(6) 0.030(3) 0.040(3) 0.042(3) -0.001(3) 0.008(2) 0.003(2) C(7) 0.044(4) 0.049(4) 0.053(4) 0.004(3) 0.008(3) 0.003(3) C(8) 0.069(5) 0.053(4) 0.080(5) 0.011(4) 0.027(4) 0.020(4) C(9) 0.061(5) 0.080(5) 0.042(4) 0.008(4) 0.006(3) 0.019(3) C(10) 0.059(4) 0.058(5) 0.035(3) 0.004(3) 0.016(3) -0.003(3) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3342 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0480 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0593 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.625 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.89 _refine_diff_density_max 0.74 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr(1) O(1) 2.442(4) ? ? yes Pr(1) O(2) 2.388(4) ? ? yes Pr(1) O(2) 2.429(4) ? ? yes Pr(1) O(3) 2.622(4) ? ? yes Pr(1) O(4) 2.585(4) ? ? yes Pr(1) O(6) 2.612(4) ? ? yes Pr(1) O(7) 2.529(5) ? ? yes Pr(1) O(9) 2.467(4) ? ? yes Pr(1) O(10) 2.542(5) ? ? yes O(1) C(4) 1.276(6) ? ? yes O(2) C(6) 1.358(6) ? ? yes O(3) N(3) 1.256(6) ? ? yes O(4) N(3) 1.264(7) ? ? yes O(5) N(3) 1.224(7) ? ? yes O(6) N(4) 1.280(9) ? ? yes O(7) N(4) 1.268(8) ? ? yes O(8) N(4) 1.230(8) ? ? yes O(11) N(5) 1.226(9) ? ? yes O(12) N(5) 1.240(9) ? ? yes O(13) N(5) 1.24(1) ? ? yes N(1) C(1) 1.496(9) ? ? yes N(1) C(2) 1.523(8) ? ? yes N(2) C(3) 1.461(9) ? ? yes N(2) C(4) 1.338(8) ? ? yes N(6) C(12) 1.12(1) ? ? yes N(7) C(14) 1.12(1) ? ? yes C(1) C(1) 1.51(1) ? ? yes C(2) C(3) 1.52(1) ? ? yes C(4) C(5) 1.485(8) ? ? yes C(5) C(6) 1.402(9) ? ? yes C(5) C(10) 1.375(9) ? ? yes C(6) C(7) 1.375(8) ? ? yes C(7) C(8) 1.390(10) ? ? yes C(8) C(9) 1.37(1) ? ? yes C(9) C(10) 1.38(1) ? ? yes C(11) C(12) 1.36(1) ? ? yes C(13) C(14) 1.45(2) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Pr(1) O(2) 120.9(1) ? ? ? yes O(1) Pr(1) O(2) 69.7(1) ? ? ? yes O(1) Pr(1) O(3) 71.1(1) ? ? ? yes O(1) Pr(1) O(4) 111.1(1) ? ? ? yes O(1) Pr(1) O(6) 119.1(1) ? ? ? yes O(1) Pr(1) O(7) 78.9(1) ? ? ? yes O(1) Pr(1) O(9) 142.5(2) ? ? ? yes O(1) Pr(1) O(10) 67.9(1) ? ? ? yes O(2) Pr(1) O(2) 66.4(1) ? ? ? yes O(2) Pr(1) O(3) 74.6(1) ? ? ? yes O(2) Pr(1) O(4) 76.5(1) ? ? ? yes O(2) Pr(1) O(6) 83.4(1) ? ? ? yes O(2) Pr(1) O(7) 130.8(1) ? ? ? yes O(2) Pr(1) O(9) 95.7(1) ? ? ? yes O(2) Pr(1) O(10) 148.0(1) ? ? ? yes O(2) Pr(1) O(3) 94.0(1) ? ? ? yes O(2) Pr(1) O(4) 133.9(1) ? ? ? yes O(2) Pr(1) O(6) 73.4(1) ? ? ? yes O(2) Pr(1) O(7) 83.6(1) ? ? ? yes O(2) Pr(1) O(9) 140.1(1) ? ? ? yes O(2) Pr(1) O(10) 136.6(1) ? ? ? yes O(3) Pr(1) O(4) 48.9(1) ? ? ? yes O(3) Pr(1) O(6) 157.7(2) ? ? ? yes O(3) Pr(1) O(7) 148.7(1) ? ? ? yes O(3) Pr(1) O(9) 116.2(1) ? ? ? yes O(3) Pr(1) O(10) 80.9(2) ? ? ? yes O(4) Pr(1) O(6) 129.4(1) ? ? ? yes O(4) Pr(1) O(7) 142.5(1) ? ? ? yes O(4) Pr(1) O(9) 67.4(1) ? ? ? yes O(4) Pr(1) O(10) 71.9(1) ? ? ? yes O(6) Pr(1) O(7) 49.9(2) ? ? ? yes O(6) Pr(1) O(9) 69.1(1) ? ? ? yes O(6) Pr(1) O(10) 120.9(2) ? ? ? yes O(7) Pr(1) O(9) 82.8(1) ? ? ? yes O(7) Pr(1) O(10) 79.8(2) ? ? ? yes O(9) Pr(1) O(10) 76.8(1) ? ? ? yes Pr(1) O(1) C(4) 131.4(4) ? ? ? yes Pr(1) O(2) Pr(1) 110.0(1) ? ? ? yes Pr(1) O(2) C(6) 131.1(3) ? ? ? yes Pr(1) O(2) C(6) 118.8(4) ? ? ? yes Pr(1) O(3) N(3) 95.9(3) ? ? ? yes Pr(1) O(4) N(3) 97.5(3) ? ? ? yes Pr(1) O(6) N(4) 94.3(3) ? ? ? yes Pr(1) O(7) N(4) 98.7(4) ? ? ? yes C(1) N(1) C(2) 110.2(5) ? ? ? yes C(3) N(2) C(4) 123.3(5) ? ? ? yes O(3) N(3) O(4) 117.6(5) ? ? ? yes O(3) N(3) O(5) 120.8(5) ? ? ? yes O(4) N(3) O(5) 121.6(5) ? ? ? yes O(6) N(4) O(7) 116.8(5) ? ? ? yes O(6) N(4) O(8) 121.8(6) ? ? ? yes O(7) N(4) O(8) 121.4(6) ? ? ? yes O(11) N(5) O(12) 119.5(8) ? ? ? yes O(11) N(5) O(13) 122.2(7) ? ? ? yes O(12) N(5) O(13) 118.4(7) ? ? ? yes N(1) C(1) C(1) 114.7(5) ? ? ? yes N(1) C(2) C(3) 113.3(5) ? ? ? yes N(2) C(3) C(2) 112.7(6) ? ? ? yes O(1) C(4) N(2) 120.7(5) ? ? ? yes O(1) C(4) C(5) 122.3(5) ? ? ? yes N(2) C(4) C(5) 117.0(5) ? ? ? yes C(4) C(5) C(6) 119.7(5) ? ? ? yes C(4) C(5) C(10) 120.6(6) ? ? ? yes C(6) C(5) C(10) 119.7(5) ? ? ? yes O(2) C(6) C(5) 121.3(5) ? ? ? yes O(2) C(6) C(7) 119.8(5) ? ? ? yes C(5) C(6) C(7) 119.0(5) ? ? ? yes C(6) C(7) C(8) 120.5(6) ? ? ? yes C(7) C(8) C(9) 120.3(6) ? ? ? yes C(8) C(9) C(10) 119.4(6) ? ? ? yes C(5) C(10) C(9) 121.1(6) ? ? ? yes N(6) C(12) C(11) 173(1) ? ? ? yes N(7) C(14) C(13) 177(1) ? ? ? yes #------------------------------------------------------------------------------