# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Zhou, Yunshan' _publ_contact_author_email zhouys@mail.buct.edu.cn loop_ _publ_author_name 'Yunshan Zhou' 'Sheng Xu' 'Lijuan Zhang' data_bo495 _database_code_depnum_ccdc_archive 'CCDC 819916' #TrackingRef 'web_deposit_cif_file_0_Dr.zhouyunshan_1301796370.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H19.02 Eu2 N2 O20.51 P2' _chemical_formula_weight 861.34 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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' _cell_length_a 14.132(5) _cell_length_b 10.507(3) _cell_length_c 15.816(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.504(4) _cell_angle_gamma 90.00 _cell_volume 2322.6(13) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 4006 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 27.47 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1652 _exptl_absorpt_coefficient_mu 5.589 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.4011 _exptl_absorpt_correction_T_max 0.4877 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type AFC10/Saturn724+ _diffrn_measurement_method Multi-scan _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9182 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.40 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2670 _reflns_number_gt 2494 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0266P)^2^+3.6000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2670 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0242 _refine_ls_R_factor_gt 0.0204 _refine_ls_wR_factor_ref 0.0488 _refine_ls_wR_factor_gt 0.0472 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Eu1 Eu 0.439939(10) 0.221102(13) 0.436538(9) 0.00642(6) Uani 1 1 d . . . P1 P 0.20318(5) 0.39968(7) 0.40092(5) 0.00881(15) Uani 1 1 d . . . O1 O 0.29491(15) 0.3264(2) 0.41235(13) 0.0150(5) Uani 1 1 d . . . O2 O 0.23063(15) 0.5451(2) 0.40001(15) 0.0174(5) Uani 1 1 d . . . H2O H 0.1800 0.5942 0.3918 0.021 Uiso 1 1 d R . . O3 O 0.13245(16) 0.3748(2) 0.45961(14) 0.0157(5) Uani 1 1 d . . . O4 O 0.09780(16) 0.51135(19) 0.12189(13) 0.0136(4) Uani 1 1 d . . . O5 O 0.07482(14) 0.3621(2) 0.01906(13) 0.0119(4) Uani 1 1 d . . . O6 O 0.38714(15) 0.23260(19) 0.28030(14) 0.0097(4) Uani 1 1 d . . . O7 O 0.42896(14) 0.19545(19) 0.15071(13) 0.0099(4) Uani 1 1 d . . . O8 O 0.49345(16) 0.4327(2) 0.39794(14) 0.0163(5) Uani 1 1 d . . . O9 O 0.53066(16) 0.6312(2) 0.44240(13) 0.0158(5) Uani 1 1 d . . . N1 N 0.21326(18) 0.3603(2) 0.23161(15) 0.0121(5) Uani 1 1 d . . . H1A H 0.2364 0.4411 0.2255 0.015 Uiso 1 1 calc R . . H1B H 0.2641 0.3102 0.2544 0.015 Uiso 1 1 calc R . . C1 C 0.1434(2) 0.3652(3) 0.29364(19) 0.0158(7) Uani 1 1 d . . . H1C H 0.1099 0.2825 0.2936 0.019 Uiso 1 1 calc R . . H1D H 0.0951 0.4318 0.2757 0.019 Uiso 1 1 calc R . . C2 C 0.1748(3) 0.3105(3) 0.1454(2) 0.0183(7) Uani 1 1 d . . . H2A H 0.1389 0.2311 0.1520 0.022 Uiso 1 1 calc R . . H2B H 0.2290 0.2890 0.1149 0.022 Uiso 1 1 calc R . . C3 C 0.1096(2) 0.4035(3) 0.09160(18) 0.0102(6) Uani 1 1 d . . . C4 C 0.4465(2) 0.2138(2) 0.22978(19) 0.0080(6) Uani 1 1 d . . . C5 C 0.5072(2) 0.5190(3) 0.45371(19) 0.0118(6) Uani 1 1 d . . . O10 O 0.3718(4) 0.5326(5) 0.2332(3) 0.0244(14) Uani 0.489(6) 1 d P A 1 O10' O 0.3058(4) 0.5797(5) 0.1843(4) 0.0382(17) Uani 0.511(6) 1 d P A 2 O10" O 0.5000 0.5572(7) 0.2500 0.0227(17) Uani 0.511(6) 2 d SP A 3 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 Eu1 0.00722(8) 0.00610(8) 0.00578(9) -0.00014(5) 0.00043(6) 0.00064(5) P1 0.0087(3) 0.0095(3) 0.0082(4) 0.0015(3) 0.0011(3) 0.0023(3) O1 0.0141(11) 0.0212(11) 0.0099(11) 0.0022(9) 0.0023(9) 0.0103(9) O2 0.0107(11) 0.0107(11) 0.0307(13) 0.0013(10) 0.0032(10) -0.0003(8) O3 0.0194(12) 0.0136(11) 0.0161(11) 0.0048(9) 0.0093(9) 0.0045(9) O4 0.0226(12) 0.0083(10) 0.0094(10) 0.0006(8) 0.0007(9) 0.0045(9) O5 0.0102(10) 0.0144(11) 0.0101(10) -0.0022(8) -0.0013(8) -0.0020(8) O6 0.0087(10) 0.0126(10) 0.0080(11) -0.0004(8) 0.0017(8) 0.0012(8) O7 0.0100(10) 0.0129(10) 0.0065(10) -0.0002(8) 0.0003(8) -0.0019(8) O8 0.0240(12) 0.0106(11) 0.0142(11) -0.0054(9) 0.0029(9) -0.0032(9) O9 0.0245(12) 0.0107(10) 0.0121(11) -0.0011(9) 0.0022(9) -0.0038(9) N1 0.0145(13) 0.0119(13) 0.0087(12) -0.0012(10) -0.0030(10) 0.0042(10) C1 0.0117(15) 0.0225(17) 0.0130(16) 0.0012(13) 0.0010(12) -0.0017(12) C2 0.0269(18) 0.0146(15) 0.0116(16) -0.0046(13) -0.0035(14) 0.0076(13) C3 0.0112(14) 0.0125(14) 0.0076(14) -0.0003(12) 0.0037(11) -0.0005(11) C4 0.0087(14) 0.0043(12) 0.0106(15) 0.0002(11) 0.0008(12) -0.0001(10) C5 0.0123(14) 0.0105(14) 0.0122(15) -0.0019(12) 0.0010(12) 0.0011(11) O10 0.025(3) 0.025(3) 0.023(3) 0.000(2) 0.002(2) 0.002(2) O10' 0.026(3) 0.033(3) 0.056(4) 0.001(3) 0.007(3) 0.000(2) O10" 0.026(4) 0.034(4) 0.008(3) 0.000 0.004(3) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Eu1 O3 2.293(2) 7_556 ? Eu1 O1 2.311(2) . ? Eu1 O5 2.316(2) 8_556 ? Eu1 O4 2.419(2) 4_545 ? Eu1 O9 2.452(2) 5_666 ? Eu1 O8 2.454(2) . ? Eu1 O6 2.476(2) . ? Eu1 O7 2.483(2) 2_655 ? Eu1 C5 3.262(3) 5_666 ? P1 O3 1.484(2) . ? P1 O1 1.495(2) . ? P1 O2 1.578(2) . ? P1 C1 1.816(3) . ? O2 H2O 0.8761 . ? O3 Eu1 2.293(2) 7_556 ? O4 C3 1.251(4) . ? O4 Eu1 2.419(2) 4 ? O5 C3 1.257(3) . ? O5 Eu1 2.316(2) 8_455 ? O6 C4 1.257(4) . ? O7 C4 1.253(4) . ? O7 Eu1 2.483(2) 2_655 ? O8 C5 1.260(4) . ? O9 C5 1.244(4) . ? O9 Eu1 2.452(2) 5_666 ? N1 C2 1.485(4) . ? N1 C1 1.492(4) . ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? C1 H1C 0.9900 . ? C1 H1D 0.9900 . ? C2 C3 1.516(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C4 C4 1.552(6) 2_655 ? C5 C5 1.560(6) 5_666 ? C5 Eu1 3.262(3) 5_666 ? 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 O3 Eu1 O1 81.39(8) 7_556 . ? O3 Eu1 O5 81.24(8) 7_556 8_556 ? O1 Eu1 O5 155.48(7) . 8_556 ? O3 Eu1 O4 77.10(8) 7_556 4_545 ? O1 Eu1 O4 103.48(8) . 4_545 ? O5 Eu1 O4 89.32(7) 8_556 4_545 ? O3 Eu1 O9 76.15(8) 7_556 5_666 ? O1 Eu1 O9 82.52(8) . 5_666 ? O5 Eu1 O9 76.61(7) 8_556 5_666 ? O4 Eu1 O9 151.33(7) 4_545 5_666 ? O3 Eu1 O8 139.71(7) 7_556 . ? O1 Eu1 O8 79.82(8) . . ? O5 Eu1 O8 102.93(8) 8_556 . ? O4 Eu1 O8 142.09(7) 4_545 . ? O9 Eu1 O8 66.30(7) 5_666 . ? O3 Eu1 O6 129.48(8) 7_556 . ? O1 Eu1 O6 71.49(7) . . ? O5 Eu1 O6 133.01(7) 8_556 . ? O4 Eu1 O6 69.29(7) 4_545 . ? O9 Eu1 O6 137.70(7) 5_666 . ? O8 Eu1 O6 76.47(7) . . ? O3 Eu1 O7 143.04(7) 7_556 2_655 ? O1 Eu1 O7 132.56(7) . 2_655 ? O5 Eu1 O7 69.68(7) 8_556 2_655 ? O4 Eu1 O7 80.17(7) 4_545 2_655 ? O9 Eu1 O7 116.65(7) 5_666 2_655 ? O8 Eu1 O7 71.18(7) . 2_655 ? O6 Eu1 O7 65.81(7) . 2_655 ? O3 Eu1 C5 94.47(8) 7_556 5_666 ? O1 Eu1 C5 79.34(8) . 5_666 ? O5 Eu1 C5 84.90(8) 8_556 5_666 ? O4 Eu1 C5 170.45(7) 4_545 5_666 ? O9 Eu1 C5 19.22(7) 5_666 5_666 ? O8 Eu1 C5 47.11(7) . 5_666 ? O6 Eu1 C5 120.11(7) . 5_666 ? O7 Eu1 C5 104.80(7) 2_655 5_666 ? O3 P1 O1 119.05(13) . . ? O3 P1 O2 111.46(12) . . ? O1 P1 O2 106.84(13) . . ? O3 P1 C1 106.63(14) . . ? O1 P1 C1 106.57(14) . . ? O2 P1 C1 105.40(14) . . ? P1 O1 Eu1 176.66(15) . . ? P1 O2 H2O 112.0 . . ? P1 O3 Eu1 159.80(14) . 7_556 ? C3 O4 Eu1 135.51(19) . 4 ? C3 O5 Eu1 145.36(19) . 8_455 ? C4 O6 Eu1 119.72(19) . . ? C4 O7 Eu1 118.95(18) . 2_655 ? C5 O8 Eu1 119.96(19) . . ? C5 O9 Eu1 120.34(19) . 5_666 ? C2 N1 C1 115.3(3) . . ? C2 N1 H1A 108.4 . . ? C1 N1 H1A 108.4 . . ? C2 N1 H1B 108.4 . . ? C1 N1 H1B 108.4 . . ? H1A N1 H1B 107.5 . . ? N1 C1 P1 111.1(2) . . ? N1 C1 H1C 109.4 . . ? P1 C1 H1C 109.4 . . ? N1 C1 H1D 109.4 . . ? P1 C1 H1D 109.4 . . ? H1C C1 H1D 108.0 . . ? N1 C2 C3 113.5(2) . . ? N1 C2 H2A 108.9 . . ? C3 C2 H2A 108.9 . . ? N1 C2 H2B 108.9 . . ? C3 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? O4 C3 O5 127.4(3) . . ? O4 C3 C2 118.2(3) . . ? O5 C3 C2 114.4(3) . . ? O7 C4 O6 127.3(3) . . ? O7 C4 C4 116.6(3) . 2_655 ? O6 C4 C4 116.1(3) . 2_655 ? O9 C5 O8 126.7(3) . . ? O9 C5 C5 116.9(3) . 5_666 ? O8 C5 C5 116.4(3) . 5_666 ? O9 C5 Eu1 40.44(14) . 5_666 ? O8 C5 Eu1 167.0(2) . 5_666 ? C5 C5 Eu1 76.5(2) 5_666 5_666 ? 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 O3 P1 O1 Eu1 -79(3) . . . . ? O2 P1 O1 Eu1 49(3) . . . . ? C1 P1 O1 Eu1 161(2) . . . . ? O3 Eu1 O1 P1 82(2) 7_556 . . . ? O5 Eu1 O1 P1 36(3) 8_556 . . . ? O4 Eu1 O1 P1 156(2) 4_545 . . . ? O9 Eu1 O1 P1 4(2) 5_666 . . . ? O8 Eu1 O1 P1 -63(2) . . . . ? O6 Eu1 O1 P1 -142(2) . . . . ? O7 Eu1 O1 P1 -115(2) 2_655 . . . ? C5 Eu1 O1 P1 -15(2) 5_666 . . . ? O1 P1 O3 Eu1 -9.5(5) . . . 7_556 ? O2 P1 O3 Eu1 -134.5(4) . . . 7_556 ? C1 P1 O3 Eu1 110.9(4) . . . 7_556 ? O3 Eu1 O6 C4 -135.93(19) 7_556 . . . ? O1 Eu1 O6 C4 162.8(2) . . . . ? O5 Eu1 O6 C4 -16.0(2) 8_556 . . . ? O4 Eu1 O6 C4 -84.3(2) 4_545 . . . ? O9 Eu1 O6 C4 107.7(2) 5_666 . . . ? O8 Eu1 O6 C4 79.2(2) . . . . ? O7 Eu1 O6 C4 3.97(18) 2_655 . . . ? C5 Eu1 O6 C4 97.6(2) 5_666 . . . ? O3 Eu1 O8 C5 19.8(3) 7_556 . . . ? O1 Eu1 O8 C5 83.3(2) . . . . ? O5 Eu1 O8 C5 -71.9(2) 8_556 . . . ? O4 Eu1 O8 C5 -177.8(2) 4_545 . . . ? O9 Eu1 O8 C5 -3.0(2) 5_666 . . . ? O6 Eu1 O8 C5 156.5(2) . . . . ? O7 Eu1 O8 C5 -134.8(2) 2_655 . . . ? C5 Eu1 O8 C5 -1.6(3) 5_666 . . . ? C2 N1 C1 P1 169.6(2) . . . . ? O3 P1 C1 N1 -167.9(2) . . . . ? O1 P1 C1 N1 -39.8(3) . . . . ? O2 P1 C1 N1 73.5(2) . . . . ? C1 N1 C2 C3 73.9(3) . . . . ? Eu1 O4 C3 O5 -26.0(5) 4 . . . ? Eu1 O4 C3 C2 152.2(2) 4 . . . ? Eu1 O5 C3 O4 -78.9(5) 8_455 . . . ? Eu1 O5 C3 C2 102.9(4) 8_455 . . . ? N1 C2 C3 O4 3.0(4) . . . . ? N1 C2 C3 O5 -178.6(3) . . . . ? Eu1 O7 C4 O6 163.1(2) 2_655 . . . ? Eu1 O7 C4 C4 -16.7(2) 2_655 . . 2_655 ? Eu1 O6 C4 O7 167.2(2) . . . . ? Eu1 O6 C4 C4 -13.0(2) . . . 2_655 ? Eu1 O9 C5 O8 -177.2(2) 5_666 . . . ? Eu1 O9 C5 C5 3.0(4) 5_666 . . 5_666 ? Eu1 O8 C5 O9 -177.1(2) . . . . ? Eu1 O8 C5 C5 2.7(4) . . . 5_666 ? Eu1 O8 C5 Eu1 174.8(8) . . . 5_666 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.983 _refine_diff_density_min -0.605 _refine_diff_density_rms 0.114 # Attachment 'web_deposit_cif_file_1_Dr.zhouyunshan_1301796370.cif' data_bo645 _database_code_depnum_ccdc_archive 'CCDC 819917' #TrackingRef 'web_deposit_cif_file_1_Dr.zhouyunshan_1301796370.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H18.92 N2 O20.46 P2 Tb2' _chemical_formula_weight 874.35 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' P P 0.1023 0.0942 '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' _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' _cell_length_a 14.069(3) _cell_length_b 10.443(2) _cell_length_c 15.714(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.528(3) _cell_angle_gamma 90.00 _cell_volume 2283.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used 3487 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 27.47 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1666 _exptl_absorpt_coefficient_mu 6.386 _exptl_absorpt_correction_type Multi-scans _exptl_absorpt_correction_T_min 0.3615 _exptl_absorpt_correction_T_max 0.4684 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type AFC10/Saturn724+ _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7783 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2551 _reflns_number_gt 2325 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0252P)^2^+7.0600P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2551 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0277 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0505 _refine_ls_wR_factor_gt 0.0486 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 0.560314(11) 0.222338(15) 0.063907(10) 0.00540(6) Uani 1 1 d . . . P1 P 0.79595(7) 0.40082(9) 0.09764(6) 0.00808(19) Uani 1 1 d . . . O1 O 0.70382(18) 0.3283(3) 0.08730(16) 0.0137(5) Uani 1 1 d . . . O2 O 0.76945(18) 0.5478(3) 0.09812(18) 0.0166(6) Uani 1 1 d . . . H2O H 0.8213 0.5939 0.1084 0.020 Uiso 1 1 d R . . O3 O 0.86585(19) 0.3746(2) 0.03770(17) 0.0145(6) Uani 1 1 d . . . O4 O 0.92759(17) 0.3624(2) 0.48107(15) 0.0104(5) Uani 1 1 d . . . O5 O 0.90580(19) 0.5130(2) 0.37836(16) 0.0125(5) Uani 1 1 d . . . O6 O 0.61320(18) 0.2334(2) 0.21982(16) 0.0091(5) Uani 1 1 d . . . O7 O 0.57112(17) 0.1975(2) 0.34991(16) 0.0086(5) Uani 1 1 d . . . O8 O 0.50752(19) 0.4329(2) 0.10259(17) 0.0143(6) Uani 1 1 d . . . O9 O 0.46868(19) 0.6323(2) 0.05745(17) 0.0146(6) Uani 1 1 d . . . N1 N 0.7872(2) 0.3622(3) 0.26817(19) 0.0130(7) Uani 1 1 d . . . H0A H 0.7644 0.4437 0.2745 0.016 Uiso 1 1 calc R . . H0B H 0.7359 0.3121 0.2455 0.016 Uiso 1 1 calc R . . C1 C 0.8569(3) 0.3665(4) 0.2056(2) 0.0165(8) Uani 1 1 d . . . H1A H 0.8905 0.2832 0.2057 0.020 Uiso 1 1 calc R . . H1B H 0.9057 0.4335 0.2233 0.020 Uiso 1 1 calc R . . C2 C 0.8266(3) 0.3119(4) 0.3546(3) 0.0173(9) Uani 1 1 d . . . H2A H 0.8624 0.2320 0.3475 0.021 Uiso 1 1 calc R . . H2B H 0.7725 0.2904 0.3857 0.021 Uiso 1 1 calc R . . C3 C 0.8927(3) 0.4050(3) 0.4083(2) 0.0077(7) Uani 1 1 d . . . C4 C 0.5535(2) 0.2159(3) 0.2701(2) 0.0068(7) Uani 1 1 d . . . C5 C 0.4929(3) 0.5189(4) 0.0461(2) 0.0117(7) Uani 1 1 d . . . O10 O 0.6287(4) 0.5355(5) 0.2670(4) 0.0257(17) Uani 0.539(7) 1 d P A 1 O10' O 0.6950(6) 0.5803(7) 0.3182(6) 0.045(3) Uani 0.461(7) 1 d P A 2 O10" O 0.5000 0.5622(9) 0.2500 0.023(2) Uani 0.461(7) 2 d SP A 2 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 0.00567(9) 0.00497(9) 0.00563(10) 0.00011(7) 0.00109(6) -0.00083(6) P1 0.0076(4) 0.0089(4) 0.0082(5) -0.0016(3) 0.0025(4) -0.0024(3) O1 0.0113(13) 0.0193(14) 0.0102(13) -0.0011(11) 0.0004(10) -0.0082(11) O2 0.0083(13) 0.0109(13) 0.0316(16) -0.0025(12) 0.0059(12) -0.0005(10) O3 0.0173(14) 0.0103(13) 0.0185(15) -0.0039(11) 0.0116(11) -0.0042(10) O4 0.0101(13) 0.0126(13) 0.0080(13) 0.0017(10) -0.0007(10) 0.0017(9) O5 0.0203(15) 0.0087(12) 0.0082(13) 0.0001(10) 0.0010(11) -0.0055(10) O6 0.0089(12) 0.0129(12) 0.0066(13) 0.0000(10) 0.0041(10) -0.0016(10) O7 0.0082(12) 0.0096(12) 0.0079(13) -0.0001(9) 0.0013(10) 0.0026(9) O8 0.0194(14) 0.0089(13) 0.0153(14) 0.0045(11) 0.0046(11) 0.0028(10) O9 0.0216(15) 0.0068(12) 0.0160(14) 0.0016(10) 0.0043(11) 0.0025(10) N1 0.0156(16) 0.0133(16) 0.0093(16) -0.0011(12) -0.0005(13) -0.0049(12) C1 0.0113(19) 0.025(2) 0.013(2) -0.0008(16) 0.0010(15) 0.0008(15) C2 0.024(2) 0.0119(19) 0.013(2) 0.0057(15) -0.0069(17) -0.0106(15) C3 0.0111(17) 0.0079(16) 0.0044(17) 0.0005(13) 0.0018(14) 0.0016(12) C4 0.0087(17) 0.0043(15) 0.0076(19) -0.0028(13) 0.0016(14) 0.0015(12) C5 0.0091(17) 0.0120(18) 0.014(2) 0.0011(15) 0.0018(15) -0.0009(13) O10 0.028(4) 0.023(3) 0.026(3) 0.000(3) 0.003(3) -0.005(2) O10' 0.029(5) 0.028(4) 0.077(7) -0.002(4) 0.006(4) 0.003(3) O10" 0.026(5) 0.033(6) 0.009(5) 0.000 0.003(4) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 O3 2.268(3) 7_655 ? Tb1 O1 2.284(2) . ? Tb1 O4 2.290(2) 8_455 ? Tb1 O5 2.387(3) 4_645 ? Tb1 O9 2.424(3) 5_665 ? Tb1 O8 2.427(3) . ? Tb1 O6 2.455(3) . ? Tb1 O7 2.462(3) 2_655 ? P1 O3 1.485(3) . ? P1 O1 1.489(3) . ? P1 O2 1.580(3) . ? P1 C1 1.820(4) . ? O2 H2O 0.8692 . ? O3 Tb1 2.268(3) 7_655 ? O4 C3 1.257(4) . ? O4 Tb1 2.290(2) 8_556 ? O5 C3 1.246(4) . ? O5 Tb1 2.387(3) 4_655 ? O6 C4 1.249(4) . ? O7 C4 1.256(4) . ? O7 Tb1 2.462(3) 2_655 ? O8 C5 1.258(4) . ? O9 C5 1.252(4) . ? O9 Tb1 2.424(3) 5_665 ? N1 C2 1.484(5) . ? N1 C1 1.489(5) . ? N1 H0A 0.9200 . ? N1 H0B 0.9200 . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.514(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C4 C4 1.544(7) 2_655 ? C5 C5 1.544(7) 5_665 ? 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 O3 Tb1 O1 80.98(9) 7_655 . ? O3 Tb1 O4 81.22(9) 7_655 8_455 ? O1 Tb1 O4 154.91(9) . 8_455 ? O3 Tb1 O5 76.85(9) 7_655 4_645 ? O1 Tb1 O5 105.10(9) . 4_645 ? O4 Tb1 O5 87.84(9) 8_455 4_645 ? O3 Tb1 O9 76.52(9) 7_655 5_665 ? O1 Tb1 O9 82.24(9) . 5_665 ? O4 Tb1 O9 76.52(9) 8_455 5_665 ? O5 Tb1 O9 150.82(9) 4_645 5_665 ? O3 Tb1 O8 140.33(9) 7_655 . ? O1 Tb1 O8 79.45(10) . . ? O4 Tb1 O8 103.80(9) 8_455 . ? O5 Tb1 O8 141.78(9) 4_645 . ? O9 Tb1 O8 66.90(9) 5_665 . ? O3 Tb1 O6 128.37(9) 7_655 . ? O1 Tb1 O6 71.75(9) . . ? O4 Tb1 O6 133.34(9) 8_455 . ? O5 Tb1 O6 69.51(8) 4_645 . ? O9 Tb1 O6 138.27(9) 5_665 . ? O8 Tb1 O6 76.48(8) . . ? O3 Tb1 O7 143.12(8) 7_655 2_655 ? O1 Tb1 O7 132.88(9) . 2_655 ? O4 Tb1 O7 69.91(9) 8_455 2_655 ? O5 Tb1 O7 79.55(9) 4_645 2_655 ? O9 Tb1 O7 116.49(9) 5_665 2_655 ? O8 Tb1 O7 71.03(8) . 2_655 ? O6 Tb1 O7 66.25(8) . 2_655 ? O3 P1 O1 118.99(15) . . ? O3 P1 O2 111.18(15) . . ? O1 P1 O2 107.01(15) . . ? O3 P1 C1 106.87(17) . . ? O1 P1 C1 106.50(17) . . ? O2 P1 C1 105.42(18) . . ? P1 O1 Tb1 176.73(17) . . ? P1 O2 H2O 110.3 . . ? P1 O3 Tb1 160.83(16) . 7_655 ? C3 O4 Tb1 146.1(2) . 8_556 ? C3 O5 Tb1 135.8(2) . 4_655 ? C4 O6 Tb1 119.5(2) . . ? C4 O7 Tb1 118.7(2) . 2_655 ? C5 O8 Tb1 119.6(2) . . ? C5 O9 Tb1 119.9(2) . 5_665 ? C2 N1 C1 114.9(3) . . ? C2 N1 H0A 108.5 . . ? C1 N1 H0A 108.5 . . ? C2 N1 H0B 108.5 . . ? C1 N1 H0B 108.5 . . ? H0A N1 H0B 107.5 . . ? N1 C1 P1 110.8(2) . . ? N1 C1 H1A 109.5 . . ? P1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? N1 C2 C3 113.5(3) . . ? N1 C2 H2A 108.9 . . ? C3 C2 H2A 108.9 . . ? N1 C2 H2B 108.9 . . ? C3 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? O5 C3 O4 127.2(3) . . ? O5 C3 C2 118.9(3) . . ? O4 C3 C2 113.9(3) . . ? O6 C4 O7 127.0(3) . . ? O6 C4 C4 116.6(4) . 2_655 ? O7 C4 C4 116.4(4) . 2_655 ? O9 C5 O8 126.5(4) . . ? O9 C5 C5 116.8(4) . 5_665 ? O8 C5 C5 116.7(4) . 5_665 ? 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 O3 P1 O1 Tb1 -63(3) . . . . ? O2 P1 O1 Tb1 64(3) . . . . ? C1 P1 O1 Tb1 176(3) . . . . ? O3 Tb1 O1 P1 67(3) 7_655 . . . ? O4 Tb1 O1 P1 22(3) 8_455 . . . ? O5 Tb1 O1 P1 141(3) 4_645 . . . ? O9 Tb1 O1 P1 -10(3) 5_665 . . . ? O8 Tb1 O1 P1 -78(3) . . . . ? O6 Tb1 O1 P1 -157(3) . . . . ? O7 Tb1 O1 P1 -129(3) 2_655 . . . ? O1 P1 O3 Tb1 -13.3(6) . . . 7_655 ? O2 P1 O3 Tb1 -138.3(5) . . . 7_655 ? C1 P1 O3 Tb1 107.1(5) . . . 7_655 ? O3 Tb1 O6 C4 -136.6(2) 7_655 . . . ? O1 Tb1 O6 C4 161.5(3) . . . . ? O4 Tb1 O6 C4 -18.0(3) 8_455 . . . ? O5 Tb1 O6 C4 -83.9(2) 4_645 . . . ? O9 Tb1 O6 C4 107.2(3) 5_665 . . . ? O8 Tb1 O6 C4 78.4(2) . . . . ? O7 Tb1 O6 C4 3.4(2) 2_655 . . . ? O3 Tb1 O8 C5 22.0(3) 7_655 . . . ? O1 Tb1 O8 C5 83.7(3) . . . . ? O4 Tb1 O8 C5 -70.8(3) 8_455 . . . ? O5 Tb1 O8 C5 -175.2(2) 4_645 . . . ? O9 Tb1 O8 C5 -2.3(3) 5_665 . . . ? O6 Tb1 O8 C5 157.3(3) . . . . ? O7 Tb1 O8 C5 -133.5(3) 2_655 . . . ? C2 N1 C1 P1 169.4(2) . . . . ? O3 P1 C1 N1 -167.6(3) . . . . ? O1 P1 C1 N1 -39.4(3) . . . . ? O2 P1 C1 N1 74.1(3) . . . . ? C1 N1 C2 C3 74.0(4) . . . . ? Tb1 O5 C3 O4 -29.4(6) 4_655 . . . ? Tb1 O5 C3 C2 149.4(3) 4_655 . . . ? Tb1 O4 C3 O5 -78.2(6) 8_556 . . . ? Tb1 O4 C3 C2 103.0(4) 8_556 . . . ? N1 C2 C3 O5 2.2(5) . . . . ? N1 C2 C3 O4 -178.9(3) . . . . ? Tb1 O6 C4 O7 167.4(3) . . . . ? Tb1 O6 C4 C4 -12.1(3) . . . 2_655 ? Tb1 O7 C4 O6 164.2(3) 2_655 . . . ? Tb1 O7 C4 C4 -16.3(2) 2_655 . . 2_655 ? Tb1 O9 C5 O8 -177.9(3) 5_665 . . . ? Tb1 O9 C5 C5 2.7(5) 5_665 . . 5_665 ? Tb1 O8 C5 O9 -177.5(3) . . . . ? Tb1 O8 C5 C5 1.9(5) . . . 5_665 ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.438 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.135