Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Daofeng Sun' 'Rong Cao' 'Yucang Liang' 'Qian Shi' 'Maochun Hong' _publ_contact_author_name 'Prof Maochun Hong' _publ_contact_author_address ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter, Chinese Academy of Scie State Key Laboratory of Structural Fuzhou Fujian 350002 CHINA ; _publ_contact_author_email 'HMC@MS.FJIRSM.AC.CN' _publ_section_title ; Syntheses, Crystal Structures and Properties of Two Novel Lanthanide-Carboxylate Polymeric Complexes ; _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA ; data_s _database_code_CSD 173158 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H3 Gd O8' _chemical_formula_weight 408.37 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Gd' 'Gd' -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.2325(7) _cell_length_b 7.9946(8) _cell_length_c 8.7833(9) _cell_angle_alpha 65.4120(10) _cell_angle_beta 86.272(2) _cell_angle_gamma 84.377(2) _cell_volume 459.42(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 47 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 25.01 _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max .16 _exptl_crystal_size_mid .10 _exptl_crystal_size_min .08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.952 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 382 _exptl_absorpt_coefficient_mu 7.260 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .4591 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siements Smart CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 2380 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0670 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 25.01 _reflns_number_total 1596 _reflns_number_gt 1418 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Shelxl-97' _computing_publication_material 'Shelxl-97' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0675P)^2^+0.0000P] 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 1596 _refine_ls_number_parameters 176 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0499 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1098 _refine_ls_wR_factor_gt 0.1057 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 Gd Gd 0.06850(6) 0.24224(6) 0.50790(5) 0.0120(2) Uani 1 1 d . . . C1 C -0.2385(12) 0.0376(14) 0.6996(11) 0.0130(19) Uani 1 1 d . . . C2 C -0.3387(13) -0.0994(13) 0.8494(12) 0.0137(19) Uani 1 1 d . . . C3 C -0.5280(12) -0.1180(13) 0.8681(11) 0.0127(19) Uani 1 1 d . . . C4 C -0.6686(13) 0.0094(13) 0.7456(12) 0.014(2) Uani 1 1 d . . . C5 C -0.5965(13) -0.2584(13) 1.0096(11) 0.016(2) Uani 1 1 d . . . H1A H -0.7238 -0.2705 1.0222 0.019 Uiso 1 1 calc R . . C6 C -0.4792(13) -0.3823(14) 1.1338(12) 0.017(2) Uani 1 1 d . . . C7 C -0.5608(14) -0.5282(14) 1.2834(13) 0.022(2) Uani 1 1 d . . . C8 C -0.2880(12) -0.3579(13) 1.1179(11) 0.0125(19) Uani 1 1 d . . . C9 C -0.1536(14) -0.4876(13) 1.2464(12) 0.016(2) Uani 1 1 d . . . C10 C -0.2184(13) -0.2186(13) 0.9747(12) 0.0135(19) Uani 1 1 d . . . H10A H -0.0914 -0.2045 0.9621 0.016 Uiso 1 1 calc R . . O1 O -0.1622(9) -0.0111(9) 0.5908(8) 0.0156(14) Uani 1 1 d . . . O2 O -0.2148(9) 0.1961(9) 0.6923(8) 0.0181(15) Uani 1 1 d . . . O3 O -0.6105(9) 0.1333(10) 0.6087(8) 0.0201(15) Uani 1 1 d . . . O4 O -0.8373(9) -0.0012(10) 0.7785(9) 0.0208(16) Uani 1 1 d . . . O5 O -0.7197(9) -0.5655(9) 1.2940(8) 0.0190(15) Uani 1 1 d . . . O6 O -0.4440(13) -0.611(2) 1.4004(14) 0.102(6) Uani 1 1 d . . . O7 O -0.0926(11) -0.6361(10) 1.2426(9) 0.0275(18) Uani 1 1 d . . . O8 O -0.1034(10) -0.4413(9) 1.3605(8) 0.0201(15) Uani 1 1 d . . . H6A H -0.503(19) -0.728(18) 1.521(16) 0.05(4) 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 Gd 0.0128(3) 0.0090(3) 0.0130(3) -0.0037(2) 0.00101(18) -0.00010(18) C1 0.006(4) 0.022(5) 0.012(5) -0.008(4) 0.000(4) 0.001(4) C2 0.019(5) 0.009(5) 0.015(5) -0.008(4) 0.002(4) 0.002(4) C3 0.008(4) 0.014(5) 0.007(4) 0.003(4) 0.004(3) 0.001(4) C4 0.014(5) 0.012(5) 0.019(5) -0.009(4) 0.002(4) -0.001(4) C5 0.017(5) 0.012(5) 0.016(5) -0.005(4) -0.001(4) 0.007(4) C6 0.012(5) 0.016(5) 0.015(5) -0.001(4) 0.002(4) 0.001(4) C7 0.022(6) 0.015(5) 0.020(5) 0.003(4) -0.002(4) -0.008(4) C8 0.017(5) 0.010(5) 0.010(5) -0.004(4) 0.000(4) -0.001(4) C9 0.018(5) 0.011(5) 0.019(5) -0.005(4) 0.002(4) -0.004(4) C10 0.009(4) 0.014(5) 0.018(5) -0.007(4) 0.003(4) -0.003(4) O1 0.018(3) 0.012(3) 0.023(4) -0.013(3) 0.005(3) -0.005(3) O2 0.019(3) 0.010(3) 0.029(4) -0.011(3) 0.002(3) -0.004(3) O3 0.018(4) 0.017(4) 0.013(3) 0.007(3) -0.002(3) -0.003(3) O4 0.009(3) 0.020(4) 0.024(4) 0.000(3) -0.001(3) 0.004(3) O5 0.014(4) 0.014(4) 0.022(4) 0.000(3) 0.003(3) -0.006(3) O6 0.032(6) 0.133(12) 0.051(6) 0.062(7) -0.024(5) -0.041(6) O7 0.039(5) 0.016(4) 0.028(4) -0.011(3) -0.020(3) 0.016(3) O8 0.030(4) 0.010(4) 0.023(4) -0.010(3) -0.005(3) 0.001(3) _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 Gd O8 2.362(6) 2_557 ? Gd O1 2.374(6) 2_556 ? Gd O5 2.434(6) 1_664 ? Gd O7 2.445(7) 1_564 ? Gd O4 2.450(7) 1_655 ? Gd O3 2.482(7) 1_655 ? Gd O2 2.485(7) . ? Gd O8 2.548(6) 1_564 ? Gd O1 2.588(6) . ? Gd C4 2.833(10) 1_655 ? Gd C9 2.862(10) 1_564 ? Gd C1 2.894(9) . ? C1 O1 1.252(11) . ? C1 O2 1.270(12) . ? C1 C2 1.513(13) . ? C2 C3 1.384(13) . ? C2 C10 1.402(14) . ? C3 C5 1.385(12) . ? C3 C4 1.502(13) . ? C4 O4 1.238(11) . ? C4 O3 1.276(11) . ? C4 Gd 2.833(10) 1_455 ? C5 C6 1.395(13) . ? C6 C8 1.405(13) . ? C6 C7 1.482(13) . ? C7 O5 1.204(12) . ? C7 O6 1.282(14) . ? C8 C10 1.392(13) . ? C8 C9 1.506(13) . ? C9 O7 1.239(12) . ? C9 O8 1.286(12) . ? C9 Gd 2.862(10) 1_546 ? O1 Gd 2.374(6) 2_556 ? O3 Gd 2.482(7) 1_455 ? O4 Gd 2.450(7) 1_455 ? O5 Gd 2.434(6) 1_446 ? O7 Gd 2.445(7) 1_546 ? O8 Gd 2.362(6) 2_557 ? O8 Gd 2.548(6) 1_546 ? 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 O8 Gd O1 156.4(2) 2_557 2_556 ? O8 Gd O5 84.8(2) 2_557 1_664 ? O1 Gd O5 86.3(2) 2_556 1_664 ? O8 Gd O7 119.0(2) 2_557 1_564 ? O1 Gd O7 79.0(2) 2_556 1_564 ? O5 Gd O7 73.2(2) 1_664 1_564 ? O8 Gd O4 84.0(2) 2_557 1_655 ? O1 Gd O4 83.2(2) 2_556 1_655 ? O5 Gd O4 124.8(2) 1_664 1_655 ? O7 Gd O4 153.7(3) 1_564 1_655 ? O8 Gd O3 81.0(2) 2_557 1_655 ? O1 Gd O3 75.5(2) 2_556 1_655 ? O5 Gd O3 72.4(2) 1_664 1_655 ? O7 Gd O3 138.0(2) 1_564 1_655 ? O4 Gd O3 52.5(2) 1_655 1_655 ? O8 Gd O2 78.1(2) 2_557 . ? O1 Gd O2 117.1(2) 2_556 . ? O5 Gd O2 152.7(2) 1_664 . ? O7 Gd O2 96.6(2) 1_564 . ? O4 Gd O2 74.6(2) 1_655 . ? O3 Gd O2 124.6(2) 1_655 . ? O8 Gd O8 67.2(3) 2_557 1_564 ? O1 Gd O8 130.2(2) 2_556 1_564 ? O5 Gd O8 72.9(2) 1_664 1_564 ? O7 Gd O8 52.1(2) 1_564 1_564 ? O4 Gd O8 145.5(2) 1_655 1_564 ? O3 Gd O8 134.3(2) 1_655 1_564 ? O2 Gd O8 80.9(2) . 1_564 ? O8 Gd O1 127.5(2) 2_557 . ? O1 Gd O1 66.5(2) 2_556 . ? O5 Gd O1 146.8(2) 1_664 . ? O7 Gd O1 82.7(2) 1_564 . ? O4 Gd O1 72.6(2) 1_655 . ? O3 Gd O1 115.7(2) 1_655 . ? O2 Gd O1 50.8(2) . . ? O8 Gd O1 109.7(2) 1_564 . ? O8 Gd C4 82.7(2) 2_557 1_655 ? O1 Gd C4 77.1(2) 2_556 1_655 ? O5 Gd C4 99.2(2) 1_664 1_655 ? O7 Gd C4 155.3(3) 1_564 1_655 ? O4 Gd C4 25.8(2) 1_655 1_655 ? O3 Gd C4 26.7(2) 1_655 1_655 ? O2 Gd C4 99.6(2) . 1_655 ? O8 Gd C4 149.3(2) 1_564 1_655 ? O1 Gd C4 93.2(2) . 1_655 ? O8 Gd C9 93.9(3) 2_557 1_564 ? O1 Gd C9 104.3(2) 2_556 1_564 ? O5 Gd C9 72.7(2) 1_664 1_564 ? O7 Gd C9 25.5(3) 1_564 1_564 ? O4 Gd C9 161.8(3) 1_655 1_564 ? O3 Gd C9 145.1(3) 1_655 1_564 ? O2 Gd C9 87.2(2) . 1_564 ? O8 Gd C9 26.7(2) 1_564 1_564 ? O1 Gd C9 94.9(2) . 1_564 ? C4 Gd C9 171.5(3) 1_655 1_564 ? O8 Gd C1 102.0(3) 2_557 . ? O1 Gd C1 91.3(2) 2_556 . ? O5 Gd C1 167.1(2) 1_664 . ? O7 Gd C1 93.9(3) 1_564 . ? O4 Gd C1 67.3(2) 1_655 . ? O3 Gd C1 119.2(2) 1_655 . ? O2 Gd C1 25.9(2) . . ? O8 Gd C1 99.4(2) 1_564 . ? O1 Gd C1 25.6(2) . . ? C4 Gd C1 92.6(3) 1_655 . ? C9 Gd C1 95.6(3) 1_564 . ? O1 C1 O2 119.5(8) . . ? O1 C1 C2 120.0(9) . . ? O2 C1 C2 120.1(8) . . ? O1 C1 Gd 63.4(5) . . ? O2 C1 Gd 58.8(5) . . ? C2 C1 Gd 157.3(6) . . ? C3 C2 C10 120.2(9) . . ? C3 C2 C1 126.6(8) . . ? C10 C2 C1 113.2(8) . . ? C2 C3 C5 119.3(8) . . ? C2 C3 C4 124.1(8) . . ? C5 C3 C4 116.6(8) . . ? O4 C4 O3 120.5(9) . . ? O4 C4 C3 121.0(9) . . ? O3 C4 C3 118.5(8) . . ? O4 C4 Gd 59.5(5) . 1_455 ? O3 C4 Gd 61.1(5) . 1_455 ? C3 C4 Gd 178.0(7) . 1_455 ? C3 C5 C6 121.6(9) . . ? C5 C6 C8 118.9(9) . . ? C5 C6 C7 119.2(9) . . ? C8 C6 C7 121.8(9) . . ? O5 C7 O6 123.5(10) . . ? O5 C7 C6 123.6(9) . . ? O6 C7 C6 112.9(9) . . ? C10 C8 C6 119.6(9) . . ? C10 C8 C9 118.7(8) . . ? C6 C8 C9 121.6(8) . . ? O7 C9 O8 120.7(9) . . ? O7 C9 C8 120.6(9) . . ? O8 C9 C8 118.7(8) . . ? O7 C9 Gd 58.1(5) . 1_546 ? O8 C9 Gd 62.9(5) . 1_546 ? C8 C9 Gd 173.8(6) . 1_546 ? C8 C10 C2 120.3(9) . . ? C1 O1 Gd 150.9(6) . 2_556 ? C1 O1 Gd 91.0(5) . . ? Gd O1 Gd 113.5(2) 2_556 . ? C1 O2 Gd 95.3(5) . . ? C4 O3 Gd 92.1(5) . 1_455 ? C4 O4 Gd 94.7(6) . 1_455 ? C7 O5 Gd 137.8(7) . 1_446 ? C9 O7 Gd 96.4(6) . 1_546 ? C9 O8 Gd 156.7(6) . 2_557 ? C9 O8 Gd 90.4(5) . 1_546 ? Gd O8 Gd 112.8(3) 2_557 1_546 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.471 _refine_diff_density_min -2.541 _refine_diff_density_rms 0.306 data_s_2 _database_code_CSD 173159 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H5 Nd O9' _chemical_formula_weight 413.38 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Nd' 'Nd' -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.3822(5) _cell_length_b 9.3323(7) _cell_length_c 9.5201(7) _cell_angle_alpha 88.422(2) _cell_angle_beta 74.446(2) _cell_angle_gamma 76.6470(10) _cell_volume 531.13(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 39 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 25.16 _exptl_crystal_description 'block' _exptl_crystal_colour 'gray' _exptl_crystal_size_max .34 _exptl_crystal_size_mid .10 _exptl_crystal_size_min .08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 394 _exptl_absorpt_coefficient_mu 4.937 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .5687 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siements Smart CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 2784 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 25.16 _reflns_number_total 1868 _reflns_number_gt 1759 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Shelxl-97' _computing_publication_material 'Shelxl-97' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+0.0000P] 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 1868 _refine_ls_number_parameters 185 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0293 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0712 _refine_ls_wR_factor_gt 0.0706 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 Nd Nd 0.15184(3) 0.55960(2) 0.28002(2) 0.00856(12) Uani 1 1 d . . . O1 O -0.1032(6) 0.7421(4) 0.1624(4) 0.0222(8) Uani 1 1 d . . . O2 O -0.0866(7) 0.9740(4) 0.1974(5) 0.0243(9) Uani 1 1 d . . . O5 O 0.1545(5) 0.3735(4) 0.4880(4) 0.0161(7) Uani 1 1 d . . . O6 O 0.4520(5) 0.3419(3) 0.3006(3) 0.0125(7) Uani 1 1 d . . . O9 O -0.1585(7) 0.4468(5) 0.2759(5) 0.0340(10) Uani 1 1 d . . . C1 C -0.3365(8) 0.9362(5) 0.0685(5) 0.0114(9) Uani 1 1 d . . . C2 C -0.3942(8) 1.0880(5) 0.0555(5) 0.0142(10) Uani 1 1 d . . . H2A H -0.3217 1.1467 0.0938 0.017 Uiso 1 1 calc R . . C3 C -0.5565(8) 1.1548(5) -0.0127(5) 0.0121(9) Uani 1 1 d . . . C5 C 0.3353(8) 0.0374(5) 0.4285(5) 0.0115(9) Uani 1 1 d . . . H5A H 0.2238 0.0628 0.3803 0.014 Uiso 1 1 calc R . . C6 C 0.4284(7) 0.1466(5) 0.4659(5) 0.0094(9) Uani 1 1 d . . . C7 C -0.1641(8) 0.8737(5) 0.1468(5) 0.0139(10) Uani 1 1 d . . . C9 C 0.3441(7) 0.2976(5) 0.4175(5) 0.0100(9) Uani 1 1 d . . . C10 C -0.6020(8) 1.3218(5) -0.0218(5) 0.0116(9) Uani 1 1 d . . . O4 O -0.4620(6) 1.3708(4) -0.1167(4) 0.0233(8) Uani 1 1 d . . . O3 O -0.7679(6) 1.3973(4) 0.0675(4) 0.0177(7) Uani 1 1 d . . . C4 C 0.4048(8) -0.1086(5) 0.4616(5) 0.0106(9) Uani 1 1 d . . . C8 C 0.3028(7) -0.2221(5) 0.4163(5) 0.0106(9) Uani 1 1 d . . . O8 O 0.1475(6) -0.1814(4) 0.3542(4) 0.0170(7) Uani 1 1 d . . . O7 O 0.3719(6) -0.3558(4) 0.4372(4) 0.0161(7) Uani 1 1 d . . . H2B H -0.007(13) 0.931(8) 0.242(8) 0.04(2) 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 Nd 0.00878(16) 0.00597(17) 0.01180(17) 0.00227(10) -0.00487(11) -0.00117(10) O1 0.032(2) 0.0086(18) 0.035(2) 0.0028(15) -0.0265(18) -0.0012(15) O2 0.031(2) 0.0155(19) 0.037(2) 0.0060(17) -0.0275(19) -0.0061(17) O5 0.0119(17) 0.0104(17) 0.0219(18) 0.0034(14) -0.0014(14) 0.0015(13) O6 0.0138(16) 0.0095(16) 0.0135(17) 0.0054(13) -0.0033(13) -0.0022(13) O9 0.028(2) 0.054(3) 0.028(2) 0.0002(19) -0.0058(17) -0.027(2) C1 0.011(2) 0.012(2) 0.011(2) 0.0019(18) -0.0048(18) -0.0013(18) C2 0.018(2) 0.012(2) 0.016(2) 0.0026(19) -0.008(2) -0.0051(19) C3 0.013(2) 0.011(2) 0.011(2) 0.0042(17) -0.0025(18) -0.0008(18) C5 0.011(2) 0.010(2) 0.016(2) 0.0026(18) -0.0072(18) -0.0015(18) C6 0.011(2) 0.005(2) 0.011(2) 0.0004(17) -0.0042(18) 0.0020(17) C7 0.013(2) 0.016(3) 0.015(2) 0.0005(19) -0.0058(19) -0.003(2) C9 0.011(2) 0.006(2) 0.017(2) -0.0003(18) -0.0096(19) -0.0027(18) C10 0.014(2) 0.011(2) 0.015(2) 0.0001(18) -0.011(2) -0.0048(19) O4 0.027(2) 0.0187(19) 0.0227(19) 0.0035(15) 0.0027(16) -0.0128(16) O3 0.0151(17) 0.0175(18) 0.0173(18) -0.0032(14) -0.0020(14) 0.0003(14) C4 0.012(2) 0.009(2) 0.011(2) 0.0018(17) -0.0030(18) -0.0025(18) C8 0.009(2) 0.014(2) 0.009(2) -0.0003(18) -0.0027(17) -0.0027(18) O8 0.0192(18) 0.0102(17) 0.0271(19) 0.0018(14) -0.0169(16) -0.0017(14) O7 0.0215(18) 0.0060(17) 0.0260(19) 0.0048(13) -0.0152(15) -0.0033(14) _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 Nd O4 2.376(3) 2_575 ? Nd O3 2.430(3) 1_645 ? Nd O9 2.458(4) . ? Nd O6 2.493(3) . ? Nd O5 2.507(3) 2_566 ? Nd O8 2.528(3) 1_565 ? Nd O1 2.529(3) . ? Nd O7 2.557(3) 1_565 ? Nd O5 2.599(3) . ? Nd C8 2.912(4) 1_565 ? Nd C9 2.915(5) . ? O1 C7 1.217(6) . ? O2 C7 1.311(6) . ? O5 C9 1.270(6) . ? O5 Nd 2.507(3) 2_566 ? O6 C9 1.257(6) . ? C1 C2 1.390(7) . ? C1 C3 1.399(7) 2_475 ? C1 C7 1.492(7) . ? C2 C3 1.388(7) . ? C3 C1 1.399(7) 2_475 ? C3 C10 1.522(6) . ? C5 C4 1.387(7) . ? C5 C6 1.390(7) . ? C6 C4 1.394(6) 2_656 ? C6 C9 1.495(6) . ? C10 O3 1.243(6) . ? C10 O4 1.247(6) . ? O4 Nd 2.376(3) 2_575 ? O3 Nd 2.430(3) 1_465 ? C4 C6 1.394(6) 2_656 ? C4 C8 1.493(6) . ? C8 O7 1.253(6) . ? C8 O8 1.267(6) . ? C8 Nd 2.912(4) 1_545 ? O8 Nd 2.528(3) 1_545 ? O7 Nd 2.557(3) 1_545 ? 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 Nd O3 76.95(12) 2_575 1_645 ? O4 Nd O9 139.97(14) 2_575 . ? O3 Nd O9 66.76(13) 1_645 . ? O4 Nd O6 81.04(12) 2_575 . ? O3 Nd O6 72.29(11) 1_645 . ? O9 Nd O6 102.52(13) . . ? O4 Nd O5 145.45(12) 2_575 2_566 ? O3 Nd O5 136.52(11) 1_645 2_566 ? O9 Nd O5 70.06(13) . 2_566 ? O6 Nd O5 113.34(10) . 2_566 ? O4 Nd O8 72.43(12) 2_575 1_565 ? O3 Nd O8 142.26(12) 1_645 1_565 ? O9 Nd O8 130.24(13) . 1_565 ? O6 Nd O8 122.71(11) . 1_565 ? O5 Nd O8 73.51(11) 2_566 1_565 ? O4 Nd O1 88.55(13) 2_575 . ? O3 Nd O1 87.16(12) 1_645 . ? O9 Nd O1 73.80(14) . . ? O6 Nd O1 158.56(12) . . ? O5 Nd O1 85.68(12) 2_566 . ? O8 Nd O1 70.72(11) 1_565 . ? O4 Nd O7 73.38(12) 2_575 1_565 ? O3 Nd O7 137.28(11) 1_645 1_565 ? O9 Nd O7 146.29(13) . 1_565 ? O6 Nd O7 73.29(11) . 1_565 ? O5 Nd O7 80.85(11) 2_566 1_565 ? O8 Nd O7 50.94(11) 1_565 1_565 ? O1 Nd O7 121.61(11) . 1_565 ? O4 Nd O5 128.13(12) 2_575 . ? O3 Nd O5 101.92(11) 1_645 . ? O9 Nd O5 77.34(13) . . ? O6 Nd O5 51.10(10) . . ? O5 Nd O5 63.14(12) 2_566 . ? O8 Nd O5 114.19(11) 1_565 . ? O1 Nd O5 143.25(12) . . ? O7 Nd O5 74.46(11) 1_565 . ? O4 Nd C8 68.73(12) 2_575 1_565 ? O3 Nd C8 145.38(12) 1_645 1_565 ? O9 Nd C8 147.08(14) . 1_565 ? O6 Nd C8 97.38(12) . 1_565 ? O5 Nd C8 78.08(12) 2_566 1_565 ? O8 Nd C8 25.70(12) 1_565 1_565 ? O1 Nd C8 96.20(12) . 1_565 ? O7 Nd C8 25.43(12) 1_565 1_565 ? O5 Nd C8 95.79(12) . 1_565 ? O4 Nd C9 105.21(13) 2_575 . ? O3 Nd C9 85.47(12) 1_645 . ? O9 Nd C9 88.65(14) . . ? O6 Nd C9 25.37(12) . . ? O5 Nd C9 88.75(12) 2_566 . ? O8 Nd C9 123.39(11) 1_565 . ? O1 Nd C9 162.45(13) . . ? O7 Nd C9 73.67(11) 1_565 . ? O5 Nd C9 25.82(12) . . ? C8 Nd C9 98.91(12) 1_565 . ? C7 O1 Nd 141.6(3) . . ? C9 O5 Nd 151.0(3) . 2_566 ? C9 O5 Nd 91.1(3) . . ? Nd O5 Nd 116.86(12) 2_566 . ? C9 O6 Nd 96.4(3) . . ? C2 C1 C3 120.3(4) . 2_475 ? C2 C1 C7 118.6(4) . . ? C3 C1 C7 121.1(4) 2_475 . ? C3 C2 C1 122.1(5) . . ? C2 C3 C1 117.6(5) . 2_475 ? C2 C3 C10 117.0(4) . . ? C1 C3 C10 125.4(4) 2_475 . ? C4 C5 C6 121.5(4) . . ? C5 C6 C4 119.2(4) . 2_656 ? C5 C6 C9 115.5(4) . . ? C4 C6 C9 125.2(4) 2_656 . ? O1 C7 O2 123.7(5) . . ? O1 C7 C1 122.8(4) . . ? O2 C7 C1 113.5(4) . . ? O6 C9 O5 120.9(4) . . ? O6 C9 C6 119.5(4) . . ? O5 C9 C6 119.3(4) . . ? O6 C9 Nd 58.2(2) . . ? O5 C9 Nd 63.0(2) . . ? C6 C9 Nd 168.1(3) . . ? O3 C10 O4 125.7(5) . . ? O3 C10 C3 118.3(4) . . ? O4 C10 C3 116.0(4) . . ? C10 O4 Nd 170.8(4) . 2_575 ? C10 O3 Nd 138.4(3) . 1_465 ? C5 C4 C6 119.3(4) . 2_656 ? C5 C4 C8 119.4(4) . . ? C6 C4 C8 121.3(4) 2_656 . ? O7 C8 O8 120.5(4) . . ? O7 C8 C4 120.6(4) . . ? O8 C8 C4 118.9(4) . . ? O7 C8 Nd 61.2(2) . 1_545 ? O8 C8 Nd 59.9(2) . 1_545 ? C4 C8 Nd 170.5(3) . 1_545 ? C8 O8 Nd 94.4(3) . 1_545 ? C8 O7 Nd 93.3(3) . 1_545 ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.16 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.341 _refine_diff_density_min -1.901 _refine_diff_density_rms 0.185