# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2008 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Zhen-Gang Sun' _publ_contact_author_email SZG188@163.COM _publ_section_title ; Synthesis, crystal structure and luminescence property of lanthanide oxalatophosphonates with a three-dimensional framework structure ; loop_ _publ_author_name 'Zhen-Gang Sun.' 'Lei Liu.' 'Xin Lu.' 'Fei Tong.' 'Jing Zhang.' 'Na Zhang.' ; Yan Zhao ; 'Yanyu Zhu.' # Attachment '670477.cif' data_0405a _database_code_depnum_ccdc_archive 'CCDC 670477' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H9 La O11 P' _chemical_formula_weight 390.98 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.1991(6) _cell_length_b 13.3838(11) _cell_length_c 10.2926(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.8980(10) _cell_angle_gamma 90.00 _cell_volume 979.77(14) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 3490 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 28.82 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.651 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 4.576 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6601 _exptl_absorpt_correction_T_max 0.8002 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Smart Apex II CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5382 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 26.49 _reflns_number_total 2017 _reflns_number_gt 1854 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0267P)^2^+1.0238P] 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 SHELXL _refine_ls_extinction_coef 0.0115(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2017 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0233 _refine_ls_R_factor_gt 0.0210 _refine_ls_wR_factor_ref 0.0561 _refine_ls_wR_factor_gt 0.0548 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 La1 La 0.84072(2) 0.094057(12) 0.717622(17) 0.01283(10) Uani 1 1 d . . . P1 P 1.21498(11) -0.05193(6) 0.92640(8) 0.01268(18) Uani 1 1 d . . . O1 O 1.3978(4) -0.08400(17) 0.8708(3) 0.0216(5) Uani 1 1 d . . . H1A H 1.4100 -0.0491 0.8072 0.032 Uiso 1 1 calc R . . O2 O 1.1353(3) 0.04476(16) 0.8685(2) 0.0187(5) Uani 1 1 d . . . O3 O 1.2569(3) -0.05794(18) 1.0732(2) 0.0209(5) Uani 1 1 d . . . O4 O 1.1496(3) -0.24478(15) 0.9240(2) 0.0174(5) Uani 1 1 d . . . H4A H 1.1265 -0.2559 0.9982 0.026 Uiso 1 1 calc R . . O5 O 0.9213(4) -0.08891(16) 0.6673(3) 0.0213(6) Uani 1 1 d . . . O6 O 1.0403(4) -0.24278(16) 0.6697(2) 0.0212(5) Uani 1 1 d . . . O7 O 0.6901(3) 0.07647(18) 0.4793(3) 0.0218(5) Uani 1 1 d . . . O8 O 0.4674(3) 0.00985(19) 0.3292(2) 0.0227(5) Uani 1 1 d . . . O9 O 1.1378(4) 0.1167(2) 0.6065(3) 0.0359(7) Uani 1 1 d . . . H9A H 1.2086 0.0660 0.6227 0.054 Uiso 1 1 d R . . H9B H 1.1049 0.1224 0.5239 0.054 Uiso 1 1 d R . . O10 O 0.5466(4) 0.2066(2) 0.7245(3) 0.0428(8) Uani 1 1 d . . . H10A H 0.4733 0.1779 0.7700 0.064 Uiso 1 1 d R . . H10B H 0.5813 0.2625 0.7593 0.064 Uiso 1 1 d R . . O1W O 0.3731(4) 0.2177(2) 0.9402(3) 0.0473(8) Uani 1 1 d . . . H1WA H 0.3865 0.1928 1.0170 0.071 Uiso 1 1 d R . . H1WB H 0.3821 0.2810 0.9456 0.071 Uiso 1 1 d R . . C1 C 1.0546(4) -0.1560(2) 0.8737(3) 0.0136(6) Uani 1 1 d . . . H1B H 0.9398 -0.1481 0.9129 0.016 Uiso 1 1 calc R . . C2 C 1.0026(4) -0.1629(2) 0.7255(3) 0.0148(6) Uani 1 1 d . . . C3 C 0.5465(5) 0.0260(2) 0.4452(3) 0.0158(7) 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 La1 0.01756(13) 0.01041(13) 0.00998(13) 0.00020(6) 0.00042(8) -0.00093(6) P1 0.0156(4) 0.0115(4) 0.0108(4) 0.0008(3) 0.0017(3) -0.0010(3) O1 0.0237(13) 0.0218(13) 0.0211(14) 0.0068(10) 0.0092(11) 0.0020(9) O2 0.0215(12) 0.0130(11) 0.0202(13) 0.0017(9) -0.0010(10) 0.0002(9) O3 0.0241(12) 0.0254(12) 0.0126(12) -0.0012(10) 0.0007(9) -0.0063(10) O4 0.0324(13) 0.0109(10) 0.0089(12) 0.0026(8) 0.0038(9) 0.0010(9) O5 0.0291(14) 0.0146(12) 0.0179(14) -0.0013(9) -0.0035(11) 0.0047(9) O6 0.0365(14) 0.0132(11) 0.0128(12) -0.0018(9) 0.0001(10) 0.0041(10) O7 0.0223(13) 0.0260(12) 0.0164(13) 0.0003(10) 0.0007(10) -0.0073(10) O8 0.0250(12) 0.0323(13) 0.0102(12) 0.0002(10) 0.0010(9) -0.0117(11) O9 0.0392(16) 0.0474(16) 0.0229(16) 0.0095(13) 0.0103(12) 0.0187(14) O10 0.0413(17) 0.0337(16) 0.058(2) 0.0120(15) 0.0212(15) 0.0095(13) O1W 0.0415(18) 0.0464(18) 0.053(2) -0.0008(16) 0.0045(15) 0.0022(15) C1 0.0158(15) 0.0110(14) 0.0143(17) 0.0000(12) 0.0032(12) 0.0014(11) C2 0.0169(15) 0.0125(15) 0.0141(17) -0.0004(12) -0.0003(12) -0.0011(12) C3 0.0199(16) 0.0134(14) 0.0136(17) -0.0019(12) 0.0013(13) -0.0007(12) _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 La1 O3 2.415(2) 3_757 ? La1 O2 2.515(2) . ? La1 O7 2.535(3) . ? La1 O6 2.557(2) 2_756 ? La1 O5 2.587(2) . ? La1 O9 2.594(3) . ? La1 O8 2.599(2) 3_656 ? La1 O10 2.609(3) . ? La1 O4 2.610(2) 2_756 ? P1 O3 1.496(2) . ? P1 O2 1.501(2) . ? P1 O1 1.574(3) . ? P1 C1 1.837(3) . ? O1 H1A 0.8200 . ? O3 La1 2.415(2) 3_757 ? O4 C1 1.427(4) . ? O4 La1 2.610(2) 2_746 ? O4 H4A 0.8200 . ? O5 C2 1.254(4) . ? O6 C2 1.262(4) . ? O6 La1 2.557(2) 2_746 ? O7 C3 1.240(4) . ? O8 C3 1.259(4) . ? O8 La1 2.599(2) 3_656 ? O9 H9A 0.8500 . ? O9 H9B 0.8500 . ? O10 H10A 0.8500 . ? O10 H10B 0.8500 . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? C1 C2 1.516(4) . ? C1 H1B 0.9800 . ? C3 C3 1.560(7) 3_656 ? 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 La1 O2 74.39(8) 3_757 . ? O3 La1 O7 134.77(8) 3_757 . ? O2 La1 O7 140.07(8) . . ? O3 La1 O6 83.68(8) 3_757 2_756 ? O2 La1 O6 75.69(7) . 2_756 ? O7 La1 O6 125.53(8) . 2_756 ? O3 La1 O5 95.40(9) 3_757 . ? O2 La1 O5 71.43(7) . . ? O7 La1 O5 78.11(8) . . ? O6 La1 O5 146.03(8) 2_756 . ? O3 La1 O9 142.17(9) 3_757 . ? O2 La1 O9 68.21(8) . . ? O7 La1 O9 80.96(9) . . ? O6 La1 O9 81.90(9) 2_756 . ? O5 La1 O9 78.27(9) . . ? O3 La1 O8 72.58(8) 3_757 3_656 ? O2 La1 O8 126.02(8) . 3_656 ? O7 La1 O8 62.98(8) . 3_656 ? O6 La1 O8 139.23(8) 2_756 3_656 ? O5 La1 O8 70.60(8) . 3_656 ? O9 La1 O8 135.96(9) . 3_656 ? O3 La1 O10 75.04(9) 3_757 . ? O2 La1 O10 138.18(9) . . ? O7 La1 O10 81.51(9) . . ? O6 La1 O10 73.19(9) 2_756 . ? O5 La1 O10 139.47(9) . . ? O9 La1 O10 132.27(9) . . ? O8 La1 O10 68.96(10) 3_656 . ? O3 La1 O4 134.41(8) 3_757 2_756 ? O2 La1 O4 117.96(7) . 2_756 ? O7 La1 O4 65.21(7) . 2_756 ? O6 La1 O4 60.76(7) 2_756 2_756 ? O5 La1 O4 130.11(8) . 2_756 ? O9 La1 O4 64.06(8) . 2_756 ? O8 La1 O4 115.73(7) 3_656 2_756 ? O10 La1 O4 68.27(9) . 2_756 ? O3 P1 O2 116.90(14) . . ? O3 P1 O1 107.62(14) . . ? O2 P1 O1 112.37(14) . . ? O3 P1 C1 106.08(14) . . ? O2 P1 C1 110.62(14) . . ? O1 P1 C1 102.03(14) . . ? P1 O1 H1A 109.5 . . ? P1 O2 La1 134.87(13) . . ? P1 O3 La1 150.45(14) . 3_757 ? C1 O4 La1 122.53(17) . 2_746 ? C1 O4 H4A 109.5 . . ? La1 O4 H4A 113.4 2_746 . ? C2 O5 La1 139.0(2) . . ? C2 O6 La1 126.7(2) . 2_746 ? C3 O7 La1 122.5(2) . . ? C3 O8 La1 121.0(2) . 3_656 ? La1 O9 H9A 109.4 . . ? La1 O9 H9B 109.3 . . ? H9A O9 H9B 109.5 . . ? La1 O10 H10A 109.2 . . ? La1 O10 H10B 109.4 . . ? H10A O10 H10B 109.5 . . ? H1WA O1W H1WB 109.5 . . ? O4 C1 C2 110.1(2) . . ? O4 C1 P1 106.3(2) . . ? C2 C1 P1 112.9(2) . . ? O4 C1 H1B 109.1 . . ? C2 C1 H1B 109.1 . . ? P1 C1 H1B 109.1 . . ? O5 C2 O6 124.7(3) . . ? O5 C2 C1 117.2(3) . . ? O6 C2 C1 118.1(3) . . ? O7 C3 O8 126.6(3) . . ? O7 C3 C3 118.1(3) . 3_656 ? O8 C3 C3 115.3(3) . 3_656 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.593 _refine_diff_density_min -0.516 _refine_diff_density_rms 0.119 # Attachment '670478.cif' data_0419a _database_code_depnum_ccdc_archive 'CCDC 670478' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H9 Ce O11 P' _chemical_formula_weight 392.19 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.2260(7) _cell_length_b 13.2918(13) _cell_length_c 10.2745(10) _cell_angle_alpha 90.00 _cell_angle_beta 99.4930(10) _cell_angle_gamma 90.00 _cell_volume 973.32(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2563 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 28.76 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.676 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 4.894 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7104 _exptl_absorpt_correction_T_max 0.9042 _exptl_absorpt_process_details sadabs _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 'Smart Apex II CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5454 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 26.75 _reflns_number_total 2058 _reflns_number_gt 1798 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0244P)^2^+0.7215P] 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 2058 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0296 _refine_ls_R_factor_gt 0.0239 _refine_ls_wR_factor_ref 0.0555 _refine_ls_wR_factor_gt 0.0526 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 Ce1 Ce 0.83856(3) 0.094439(15) 0.71823(2) 0.01310(8) Uani 1 1 d . . . P1 P 1.21372(14) -0.05061(7) 0.92755(10) 0.0132(2) Uani 1 1 d . . . O1 O 1.3963(4) -0.0818(2) 0.8731(3) 0.0222(6) Uani 1 1 d . . . H1A H 1.4076 -0.0465 0.8095 0.033 Uiso 1 1 calc R . . O2 O 1.1323(4) 0.04597(19) 0.8681(3) 0.0182(6) Uani 1 1 d . . . O3 O 1.2562(4) -0.0562(2) 1.0753(3) 0.0198(6) Uani 1 1 d . . . O4 O 1.1517(4) -0.24519(19) 0.9245(3) 0.0185(6) Uani 1 1 d . . . H4A H 1.1295 -0.2570 0.9987 0.028 Uiso 1 1 calc R . . O5 O 0.9207(4) -0.08803(19) 0.6663(3) 0.0221(6) Uani 1 1 d . . . O6 O 1.0396(4) -0.2430(2) 0.6693(3) 0.0221(6) Uani 1 1 d . . . O7 O 0.6913(4) 0.0752(2) 0.4806(3) 0.0211(6) Uani 1 1 d . . . O8 O 0.4676(4) 0.0089(2) 0.3282(3) 0.0242(6) Uani 1 1 d . . . O9 O 1.1290(4) 0.1144(2) 0.6072(3) 0.0347(8) Uani 1 1 d . . . H9A H 1.1999 0.0637 0.6234 0.052 Uiso 1 1 d R . . H9B H 1.0962 0.1201 0.5246 0.052 Uiso 1 1 d R . . O10 O 0.5502(5) 0.2068(3) 0.7236(4) 0.0441(9) Uani 1 1 d . . . H10A H 0.4769 0.1780 0.7691 0.066 Uiso 1 1 d R . . H10B H 0.5850 0.2627 0.7583 0.066 Uiso 1 1 d R . . O1W O 0.3767(5) 0.2195(3) 0.9375(4) 0.0491(10) Uani 1 1 d . . . H1WA H 0.3901 0.1946 1.0144 0.074 Uiso 1 1 d R . . H1WB H 0.3856 0.2828 0.9429 0.074 Uiso 1 1 d R . . C1 C 1.0549(5) -0.1559(3) 0.8745(4) 0.0143(8) Uani 1 1 d . . . H1B H 0.9410 -0.1487 0.9139 0.017 Uiso 1 1 calc R . . C2 C 1.0011(5) -0.1627(3) 0.7255(4) 0.0164(8) Uani 1 1 d . . . C3 C 0.5460(5) 0.0253(3) 0.4451(4) 0.0161(8) 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 Ce1 0.01703(13) 0.01202(12) 0.00966(12) 0.00012(8) 0.00047(8) -0.00077(9) P1 0.0157(5) 0.0126(5) 0.0109(5) 0.0005(4) 0.0015(4) -0.0010(4) O1 0.0229(15) 0.0245(16) 0.0213(16) 0.0077(12) 0.0103(12) 0.0023(12) O2 0.0228(15) 0.0109(13) 0.0194(15) -0.0007(11) -0.0012(11) -0.0007(11) O3 0.0235(15) 0.0237(15) 0.0115(14) -0.0005(11) 0.0010(11) -0.0060(12) O4 0.0302(16) 0.0119(13) 0.0132(14) 0.0029(11) 0.0028(11) 0.0029(11) O5 0.0317(16) 0.0143(14) 0.0176(15) 0.0005(11) -0.0042(12) 0.0040(12) O6 0.0370(17) 0.0152(14) 0.0129(14) -0.0016(11) 0.0005(12) 0.0041(12) O7 0.0200(15) 0.0264(16) 0.0162(15) 0.0000(12) 0.0013(11) -0.0080(12) O8 0.0242(15) 0.0344(17) 0.0132(14) 0.0009(13) 0.0006(11) -0.0114(13) O9 0.0374(19) 0.047(2) 0.0220(17) 0.0101(15) 0.0114(14) 0.0178(16) O10 0.041(2) 0.036(2) 0.059(3) 0.0118(18) 0.0192(18) 0.0110(16) O1W 0.037(2) 0.048(2) 0.062(3) -0.003(2) 0.0074(18) 0.0008(18) C1 0.019(2) 0.0117(18) 0.0127(19) -0.0021(14) 0.0046(14) -0.0017(15) C2 0.0151(19) 0.016(2) 0.017(2) -0.0017(16) -0.0014(15) -0.0018(16) C3 0.018(2) 0.0160(19) 0.014(2) -0.0023(16) 0.0022(15) 0.0021(16) _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 Ce1 O3 2.389(3) 3_757 ? Ce1 O2 2.492(3) . ? Ce1 O7 2.510(3) . ? Ce1 O6 2.538(3) 2_756 ? Ce1 O9 2.562(3) . ? Ce1 O10 2.571(3) . ? Ce1 O5 2.574(3) . ? Ce1 O8 2.580(3) 3_656 ? Ce1 O4 2.595(3) 2_756 ? P1 O2 1.500(3) . ? P1 O3 1.500(3) . ? P1 O1 1.571(3) . ? P1 C1 1.835(4) . ? O1 H1A 0.8200 . ? O3 Ce1 2.389(3) 3_757 ? O4 C1 1.429(4) . ? O4 Ce1 2.595(3) 2_746 ? O4 H4A 0.8200 . ? O5 C2 1.256(4) . ? O6 C2 1.266(4) . ? O6 Ce1 2.538(3) 2_746 ? O7 C3 1.245(5) . ? O8 C3 1.260(5) . ? O8 Ce1 2.580(3) 3_656 ? O9 H9A 0.8463 . ? O9 H9B 0.8462 . ? O10 H10A 0.8527 . ? O10 H10B 0.8443 . ? O1W H1WA 0.8468 . ? O1W H1WB 0.8442 . ? C1 C2 1.519(5) . ? C1 H1B 0.9800 . ? C3 C3 1.554(7) 3_656 ? 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 Ce1 O2 74.69(9) 3_757 . ? O3 Ce1 O7 134.80(9) 3_757 . ? O2 Ce1 O7 139.07(9) . . ? O3 Ce1 O6 84.57(9) 3_757 2_756 ? O2 Ce1 O6 75.10(9) . 2_756 ? O7 Ce1 O6 126.09(9) . 2_756 ? O3 Ce1 O9 142.47(10) 3_757 . ? O2 Ce1 O9 67.98(10) . . ? O7 Ce1 O9 79.89(10) . . ? O6 Ce1 O9 82.32(10) 2_756 . ? O3 Ce1 O10 75.68(10) 3_757 . ? O2 Ce1 O10 138.37(11) . . ? O7 Ce1 O10 82.24(11) . . ? O6 Ce1 O10 73.59(11) 2_756 . ? O9 Ce1 O10 132.49(10) . . ? O3 Ce1 O5 95.35(10) 3_757 . ? O2 Ce1 O5 71.48(8) . . ? O7 Ce1 O5 77.15(9) . . ? O6 Ce1 O5 145.28(9) 2_756 . ? O9 Ce1 O5 76.79(10) . . ? O10 Ce1 O5 140.09(11) . . ? O3 Ce1 O8 71.85(9) 3_757 3_656 ? O2 Ce1 O8 126.40(9) . 3_656 ? O7 Ce1 O8 63.46(9) . 3_656 ? O6 Ce1 O8 139.41(10) 2_756 3_656 ? O9 Ce1 O8 135.49(10) . 3_656 ? O10 Ce1 O8 68.89(11) . 3_656 ? O5 Ce1 O8 71.36(10) . 3_656 ? O3 Ce1 O4 135.64(9) 3_757 2_756 ? O2 Ce1 O4 117.50(9) . 2_756 ? O7 Ce1 O4 65.21(8) . 2_756 ? O6 Ce1 O4 61.20(8) 2_756 2_756 ? O9 Ce1 O4 64.08(9) . 2_756 ? O10 Ce1 O4 68.44(10) . 2_756 ? O5 Ce1 O4 128.93(9) . 2_756 ? O8 Ce1 O4 115.78(9) 3_656 2_756 ? O2 P1 O3 117.12(16) . . ? O2 P1 O1 112.14(16) . . ? O3 P1 O1 107.66(16) . . ? O2 P1 C1 110.36(16) . . ? O3 P1 C1 106.02(17) . . ? O1 P1 C1 102.35(17) . . ? P1 O1 H1A 109.5 . . ? P1 O2 Ce1 135.23(15) . . ? P1 O3 Ce1 150.29(16) . 3_757 ? C1 O4 Ce1 122.4(2) . 2_746 ? C1 O4 H4A 109.5 . . ? Ce1 O4 H4A 113.3 2_746 . ? C2 O5 Ce1 138.5(2) . . ? C2 O6 Ce1 126.6(2) . 2_746 ? C3 O7 Ce1 122.7(2) . . ? C3 O8 Ce1 120.4(2) . 3_656 ? Ce1 O9 H9A 110.1 . . ? Ce1 O9 H9B 109.9 . . ? H9A O9 H9B 109.2 . . ? Ce1 O10 H10A 109.3 . . ? Ce1 O10 H10B 109.6 . . ? H10A O10 H10B 109.3 . . ? H1WA O1W H1WB 109.4 . . ? O4 C1 C2 110.0(3) . . ? O4 C1 P1 106.4(2) . . ? C2 C1 P1 112.8(3) . . ? O4 C1 H1B 109.2 . . ? C2 C1 H1B 109.2 . . ? P1 C1 H1B 109.2 . . ? O5 C2 O6 124.4(4) . . ? O5 C2 C1 117.5(3) . . ? O6 C2 C1 118.1(3) . . ? O7 C3 O8 126.6(4) . . ? O7 C3 C3 117.3(4) . 3_656 ? O8 C3 C3 116.0(4) . 3_656 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.75 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.662 _refine_diff_density_min -0.714 _refine_diff_density_rms 0.134 # Attachment '670479.cif' data_0412h _database_code_depnum_ccdc_archive 'CCDC 670479' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H9 O11 P Pr' _chemical_formula_weight 392.98 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.2300(7) _cell_length_b 13.2239(13) _cell_length_c 10.2535(10) _cell_angle_alpha 90.00 _cell_angle_beta 99.8690(10) _cell_angle_gamma 90.00 _cell_volume 965.82(16) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 2854 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 28.80 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.703 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 5.263 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6003 _exptl_absorpt_correction_T_max 0.9159 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Smart Apex II CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5260 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 26.50 _reflns_number_total 1984 _reflns_number_gt 1762 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0390P)^2^+0.3344P] 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 1984 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0318 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0753 _refine_ls_wR_factor_gt 0.0726 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.003 _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 Pr1 Pr 0.83761(3) 0.094542(17) 0.71834(2) 0.01115(11) Uani 1 1 d . . . P1 P 1.21308(16) -0.04994(8) 0.92834(11) 0.0111(2) Uani 1 1 d . . . O1 O 1.3971(5) -0.0808(3) 0.8750(4) 0.0212(8) Uani 1 1 d . . . H1A H 1.4083 -0.0454 0.8111 0.032 Uiso 1 1 calc R . . O2 O 1.1313(4) 0.0469(2) 0.8685(3) 0.0167(7) Uani 1 1 d . . . O3 O 1.2552(5) -0.0554(3) 1.0765(3) 0.0182(7) Uani 1 1 d . . . O4 O 1.1532(5) -0.2462(2) 0.9245(3) 0.0163(7) Uani 1 1 d . . . H4A H 1.1315 -0.2584 0.9988 0.024 Uiso 1 1 calc R . . O5 O 0.9194(5) -0.0876(2) 0.6663(3) 0.0192(8) Uani 1 1 d . . . O6 O 1.0396(5) -0.2435(2) 0.6690(3) 0.0188(7) Uani 1 1 d . . . O7 O 0.6933(5) 0.0736(3) 0.4810(3) 0.0192(7) Uani 1 1 d . . . O8 O 0.4680(5) 0.0087(3) 0.3283(3) 0.0214(7) Uani 1 1 d . . . O9 O 1.1243(6) 0.1127(3) 0.6081(4) 0.0321(10) Uani 1 1 d . . . H9A H 1.1952 0.0620 0.6243 0.048 Uiso 1 1 d R . . H9B H 1.0914 0.1184 0.5255 0.048 Uiso 1 1 d R . . O10 O 0.5534(6) 0.2069(3) 0.7227(4) 0.0419(11) Uani 1 1 d . . . H10A H 0.4801 0.1782 0.7682 0.063 Uiso 1 1 d R . . H10B H 0.5881 0.2628 0.7574 0.063 Uiso 1 1 d R . . O1W O 0.3776(6) 0.2212(4) 0.9362(5) 0.0481(12) Uani 1 1 d . . . H1WA H 0.3911 0.1963 1.0131 0.072 Uiso 1 1 d R . . H1WB H 0.3866 0.2844 0.9416 0.072 Uiso 1 1 d R . . C1 C 1.0561(6) -0.1557(3) 0.8749(4) 0.0130(9) Uani 1 1 d . . . H1B H 0.9422 -0.1488 0.9140 0.016 Uiso 1 1 calc R . . C2 C 1.0018(6) -0.1633(3) 0.7257(4) 0.0140(9) Uani 1 1 d . . . C3 C 0.5478(6) 0.0243(3) 0.4458(4) 0.0136(9) 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 Pr1 0.01404(17) 0.00923(17) 0.00980(16) 0.00006(8) 0.00098(10) -0.00084(8) P1 0.0132(5) 0.0105(6) 0.0098(5) 0.0003(4) 0.0020(4) -0.0017(4) O1 0.0205(19) 0.0231(19) 0.0228(19) 0.0088(14) 0.0113(15) 0.0025(14) O2 0.0167(16) 0.0104(17) 0.0212(17) 0.0006(13) -0.0017(13) -0.0016(13) O3 0.0196(18) 0.0248(19) 0.0098(16) -0.0013(13) 0.0017(13) -0.0059(14) O4 0.0258(18) 0.0107(15) 0.0123(15) 0.0027(12) 0.0029(13) 0.0011(13) O5 0.0272(19) 0.0099(17) 0.0172(18) 0.0001(12) -0.0050(14) 0.0031(13) O6 0.0323(19) 0.0124(16) 0.0109(15) -0.0024(12) 0.0020(13) 0.0039(14) O7 0.0176(18) 0.0240(17) 0.0157(17) -0.0001(14) 0.0020(13) -0.0059(14) O8 0.0219(18) 0.030(2) 0.0113(16) 0.0008(14) 0.0000(13) -0.0125(15) O9 0.032(2) 0.044(2) 0.023(2) 0.0098(17) 0.0104(17) 0.0196(19) O10 0.036(2) 0.038(2) 0.057(3) 0.012(2) 0.021(2) 0.0091(19) O1W 0.036(3) 0.043(3) 0.065(3) -0.001(2) 0.008(2) 0.003(2) C1 0.015(2) 0.012(2) 0.012(2) 0.0003(16) 0.0035(16) -0.0018(17) C2 0.015(2) 0.012(2) 0.014(2) 0.0005(17) 0.0006(17) -0.0031(18) C3 0.015(2) 0.012(2) 0.013(2) -0.0045(17) 0.0001(17) -0.0024(18) _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 Pr1 O3 2.372(3) 3_757 ? Pr1 O2 2.481(3) . ? Pr1 O7 2.493(3) . ? Pr1 O6 2.522(3) 2_756 ? Pr1 O5 2.559(3) . ? Pr1 O4 2.573(3) 2_756 ? Pr1 O8 2.571(3) 3_656 ? Pr1 O10 2.542(4) . ? Pr1 O9 2.537(4) . ? P1 O2 1.498(3) . ? P1 O3 1.499(3) . ? P1 O1 1.577(4) . ? P1 C1 1.826(4) . ? O1 H1A 0.8200 . ? O3 Pr1 2.372(3) 3_757 ? O4 C1 1.435(5) . ? O4 Pr1 2.573(3) 2_746 ? O4 H4A 0.8200 . ? O5 C2 1.265(5) . ? O6 C2 1.262(5) . ? O6 Pr1 2.522(3) 2_746 ? O7 C3 1.238(5) . ? O8 C3 1.260(5) . ? O8 Pr1 2.571(3) 3_656 ? O9 H9A 0.8430 . ? O9 H9B 0.8430 . ? O10 H10A 0.8533 . ? O10 H10B 0.8401 . ? O1W H1WA 0.8441 . ? O1W H1WB 0.8399 . ? C1 C2 1.517(6) . ? C1 H1B 0.9800 . ? C3 C3 1.545(9) 3_656 ? 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 Pr1 O2 74.73(11) 3_757 . ? O3 Pr1 O7 134.96(11) 3_757 . ? O2 Pr1 O7 138.41(11) . . ? O3 Pr1 O6 84.84(11) 3_757 2_756 ? O2 Pr1 O6 74.61(10) . 2_756 ? O7 Pr1 O6 126.65(11) . 2_756 ? O3 Pr1 O5 95.17(12) 3_757 . ? O2 Pr1 O5 71.74(11) . . ? O7 Pr1 O5 76.40(11) . . ? O6 Pr1 O5 145.04(12) 2_756 . ? O3 Pr1 O4 136.25(11) 3_757 2_756 ? O2 Pr1 O4 117.27(10) . 2_756 ? O7 Pr1 O4 65.32(10) . 2_756 ? O6 Pr1 O4 61.58(10) 2_756 2_756 ? O5 Pr1 O4 128.51(11) . 2_756 ? O3 Pr1 O8 71.61(10) 3_757 3_656 ? O2 Pr1 O8 126.70(11) . 3_656 ? O7 Pr1 O8 63.71(10) . 3_656 ? O6 Pr1 O8 139.46(11) 2_756 3_656 ? O5 Pr1 O8 71.53(12) . 3_656 ? O4 Pr1 O8 115.71(10) 2_756 3_656 ? O3 Pr1 O10 76.10(12) 3_757 . ? O2 Pr1 O10 138.25(12) . . ? O7 Pr1 O10 82.97(13) . . ? O6 Pr1 O10 73.61(13) 2_756 . ? O5 Pr1 O10 140.38(13) . . ? O4 Pr1 O10 68.36(12) 2_756 . ? O8 Pr1 O10 69.03(14) 3_656 . ? O3 Pr1 O9 142.45(12) 3_757 . ? O2 Pr1 O9 67.83(11) . . ? O7 Pr1 O9 79.20(12) . . ? O6 Pr1 O9 82.73(13) 2_756 . ? O5 Pr1 O9 76.14(12) . . ? O4 Pr1 O9 64.28(11) 2_756 . ? O8 Pr1 O9 135.15(12) 3_656 . ? O10 Pr1 O9 132.61(13) . . ? O2 P1 O3 117.0(2) . . ? O2 P1 O1 112.11(19) . . ? O3 P1 O1 107.6(2) . . ? O2 P1 C1 110.55(19) . . ? O3 P1 C1 105.97(19) . . ? O1 P1 C1 102.5(2) . . ? P1 O1 H1A 109.4 . . ? P1 O2 Pr1 135.00(18) . . ? P1 O3 Pr1 150.4(2) . 3_757 ? C1 O4 Pr1 122.6(2) . 2_746 ? C1 O4 H4A 109.3 . . ? Pr1 O4 H4A 113.4 2_746 . ? C2 O5 Pr1 138.6(3) . . ? C2 O6 Pr1 126.2(3) . 2_746 ? C3 O7 Pr1 122.4(3) . . ? C3 O8 Pr1 120.2(3) . 3_656 ? Pr1 O9 H9A 110.6 . . ? Pr1 O9 H9B 110.2 . . ? H9A O9 H9B 109.0 . . ? Pr1 O10 H10A 109.2 . . ? Pr1 O10 H10B 109.8 . . ? H10A O10 H10B 109.2 . . ? H1WA O1W H1WB 109.4 . . ? O4 C1 C2 109.2(3) . . ? O4 C1 P1 106.9(3) . . ? C2 C1 P1 113.2(3) . . ? O4 C1 H1B 109.3 . . ? C2 C1 H1B 109.1 . . ? P1 C1 H1B 109.1 . . ? O5 C2 O6 124.3(4) . . ? O5 C2 C1 116.9(4) . . ? O6 C2 C1 118.7(4) . . ? O7 C3 O8 126.3(4) . . ? O7 C3 C3 118.1(5) . 3_656 ? O8 C3 C3 115.6(5) . 3_656 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.862 _refine_diff_density_min -1.211 _refine_diff_density_rms 0.200 # Attachment '670480.cif' data_0426b _database_code_depnum_ccdc_archive 'CCDC 670480' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H9 Nd O11 P' _chemical_formula_weight 396.31 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' P P 0.1023 0.0942 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.2326(6) _cell_length_b 13.1558(11) _cell_length_c 10.2337(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.1070(10) _cell_angle_gamma 90.00 _cell_volume 958.63(14) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 3662 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 29.11 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 5.636 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5255 _exptl_absorpt_correction_T_max 0.6053 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Smart Apex II CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5247 _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_sigmaI/netI 0.0276 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 3 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 26.50 _reflns_number_total 1976 _reflns_number_gt 1848 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0278P)^2^+1.9917P] 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 1976 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0242 _refine_ls_R_factor_gt 0.0220 _refine_ls_wR_factor_ref 0.0557 _refine_ls_wR_factor_gt 0.0543 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 Nd1 Nd 0.83700(3) 0.094506(15) 0.71813(2) 0.01119(10) Uani 1 1 d . . . P1 P 1.21255(16) -0.04946(8) 0.92931(10) 0.0113(2) Uani 1 1 d . . . O1 O 1.3963(5) -0.0804(2) 0.8759(3) 0.0211(7) Uani 1 1 d . . . H1A H 1.4071 -0.0447 0.8120 0.032 Uiso 1 1 calc R . . O2 O 1.1304(5) 0.0477(2) 0.8686(3) 0.0168(6) Uani 1 1 d . . . O3 O 1.2546(5) -0.0544(2) 1.0777(3) 0.0183(7) Uani 1 1 d . . . O4 O 1.1539(5) -0.2464(2) 0.9252(3) 0.0152(6) Uani 1 1 d . . . H4A H 1.1321 -0.2586 0.9996 0.023 Uiso 1 1 calc R . . O5 O 0.9191(5) -0.0874(2) 0.6662(3) 0.0205(7) Uani 1 1 d . . . O6 O 1.0391(5) -0.2442(2) 0.6694(3) 0.0191(7) Uani 1 1 d . . . O7 O 0.6949(5) 0.0731(2) 0.4814(3) 0.0176(6) Uani 1 1 d . . . O8 O 0.4672(5) 0.0086(3) 0.3280(3) 0.0224(7) Uani 1 1 d . . . O9 O 1.1213(6) 0.1114(3) 0.6083(4) 0.0304(9) Uani 1 1 d . . . H9A H 1.1922 0.0607 0.6245 0.046 Uiso 1 1 d R . . H9B H 1.0885 0.1171 0.5257 0.046 Uiso 1 1 d R . . O10 O 0.5554(6) 0.2069(3) 0.7224(4) 0.0405(10) Uani 1 1 d . . . H10A H 0.4821 0.1781 0.7679 0.061 Uiso 1 1 d R . . H10B H 0.5901 0.2628 0.7572 0.061 Uiso 1 1 d R . . O1W O 0.3789(6) 0.2221(4) 0.9343(5) 0.0497(11) Uani 1 1 d . . . H1WA H 0.3923 0.1972 1.0111 0.075 Uiso 1 1 d R . . H1WB H 0.3878 0.2853 0.9397 0.075 Uiso 1 1 d R . . C1 C 1.0559(6) -0.1562(3) 0.8748(4) 0.0120(8) Uani 1 1 d . . . H1B H 0.9423 -0.1495 0.9140 0.014 Uiso 1 1 calc R . . C2 C 1.0003(6) -0.1634(3) 0.7255(4) 0.0137(8) Uani 1 1 d . . . C3 C 0.5469(6) 0.0243(3) 0.4447(4) 0.0142(8) 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 Nd1 0.01422(15) 0.01062(14) 0.00814(13) 0.00006(7) 0.00032(9) -0.00085(8) P1 0.0135(5) 0.0114(5) 0.0088(5) 0.0000(4) 0.0012(4) -0.0013(4) O1 0.0210(18) 0.0241(17) 0.0208(17) 0.0077(13) 0.0104(14) 0.0020(14) O2 0.0193(16) 0.0117(14) 0.0177(15) 0.0020(11) -0.0014(13) 0.0003(12) O3 0.0204(17) 0.0239(16) 0.0102(15) 0.0002(12) 0.0011(13) -0.0051(13) O4 0.0245(17) 0.0111(13) 0.0097(13) 0.0028(10) 0.0026(12) 0.0015(12) O5 0.0270(19) 0.0155(16) 0.0162(16) 0.0004(11) -0.0036(14) 0.0036(13) O6 0.032(2) 0.0130(14) 0.0110(14) -0.0008(11) 0.0007(13) 0.0037(13) O7 0.0182(17) 0.0214(15) 0.0130(15) -0.0008(12) 0.0019(13) -0.0052(13) O8 0.0248(18) 0.0326(18) 0.0089(14) 0.0005(12) 0.0006(13) -0.0109(15) O9 0.032(2) 0.043(2) 0.0170(18) 0.0084(15) 0.0068(16) 0.0168(19) O10 0.038(2) 0.036(2) 0.051(3) 0.0125(18) 0.018(2) 0.0103(18) O1W 0.035(3) 0.051(3) 0.063(3) -0.001(2) 0.008(2) 0.001(2) C1 0.014(2) 0.0108(19) 0.0110(19) -0.0009(14) 0.0017(16) 0.0009(15) C2 0.013(2) 0.0110(19) 0.016(2) -0.0002(15) -0.0007(17) -0.0012(16) C3 0.018(2) 0.0140(19) 0.0109(19) -0.0014(15) 0.0031(17) 0.0006(17) _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 Nd1 O3 2.360(3) 3_757 ? Nd1 O2 2.471(3) . ? Nd1 O7 2.476(3) . ? Nd1 O6 2.504(3) 2_756 ? Nd1 O5 2.545(3) . ? Nd1 O4 2.563(3) 2_756 ? Nd1 O8 2.557(3) 3_656 ? Nd1 O10 2.523(4) . ? Nd1 O9 2.520(4) . ? P1 O2 1.498(3) . ? P1 O3 1.497(3) . ? P1 O1 1.577(3) . ? P1 C1 1.829(4) . ? O1 H1A 0.8200 . ? O3 Nd1 2.360(3) 3_757 ? O4 C1 1.431(5) . ? O4 Nd1 2.563(3) 2_746 ? O4 H4A 0.8200 . ? O5 C2 1.260(5) . ? O6 C2 1.263(5) . ? O6 Nd1 2.504(3) 2_746 ? O7 C3 1.248(5) . ? O8 C3 1.249(5) . ? O8 Nd1 2.557(3) 3_656 ? O9 H9A 0.8399 . ? O9 H9B 0.8404 . ? O10 H10A 0.8531 . ? O10 H10B 0.8361 . ? O1W H1WA 0.8417 . ? O1W H1WB 0.8356 . ? C1 C2 1.513(5) . ? C1 H1B 0.9800 . ? C3 C3 1.555(8) 3_656 ? 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 Nd1 O2 74.73(11) 3_757 . ? O3 Nd1 O7 135.08(11) 3_757 . ? O2 Nd1 O7 138.14(11) . . ? O3 Nd1 O6 85.16(10) 3_757 2_756 ? O2 Nd1 O6 74.08(10) . 2_756 ? O7 Nd1 O6 126.87(10) . 2_756 ? O3 Nd1 O5 94.99(11) 3_757 . ? O2 Nd1 O5 71.91(10) . . ? O7 Nd1 O5 76.14(10) . . ? O6 Nd1 O5 144.63(11) 2_756 . ? O3 Nd1 O4 136.76(10) 3_757 2_756 ? O2 Nd1 O4 117.02(10) . 2_756 ? O7 Nd1 O4 65.23(10) . 2_756 ? O6 Nd1 O4 61.83(9) 2_756 2_756 ? O5 Nd1 O4 128.18(10) . 2_756 ? O3 Nd1 O8 71.28(10) 3_757 3_656 ? O2 Nd1 O8 126.87(10) . 3_656 ? O7 Nd1 O8 64.08(10) . 3_656 ? O6 Nd1 O8 139.60(11) 2_756 3_656 ? O5 Nd1 O8 71.76(12) . 3_656 ? O4 Nd1 O8 115.80(10) 2_756 3_656 ? O3 Nd1 O10 76.26(12) 3_757 . ? O2 Nd1 O10 137.96(12) . . ? O7 Nd1 O10 83.46(13) . . ? O6 Nd1 O10 73.76(13) 2_756 . ? O5 Nd1 O10 140.66(13) . . ? O4 Nd1 O10 68.51(11) 2_756 . ? O8 Nd1 O10 69.09(13) 3_656 . ? O3 Nd1 O9 142.41(12) 3_757 . ? O2 Nd1 O9 67.73(11) . . ? O7 Nd1 O9 78.74(12) . . ? O6 Nd1 O9 82.89(12) 2_756 . ? O5 Nd1 O9 75.58(12) . . ? O4 Nd1 O9 64.40(11) 2_756 . ? O8 Nd1 O9 135.00(12) 3_656 . ? O10 Nd1 O9 132.88(12) . . ? O2 P1 O3 116.97(18) . . ? O2 P1 O1 111.92(18) . . ? O3 P1 O1 107.9(2) . . ? O2 P1 C1 110.46(19) . . ? O3 P1 C1 106.28(18) . . ? O1 P1 C1 102.20(19) . . ? P1 O1 H1A 109.4 . . ? P1 O2 Nd1 134.89(18) . . ? P1 O3 Nd1 150.4(2) . 3_757 ? C1 O4 Nd1 122.1(2) . 2_746 ? C1 O4 H4A 109.3 . . ? Nd1 O4 H4A 113.7 2_746 . ? C2 O5 Nd1 138.7(3) . . ? C2 O6 Nd1 126.4(3) . 2_746 ? C3 O7 Nd1 122.7(3) . . ? C3 O8 Nd1 120.2(3) . 3_656 ? Nd1 O9 H9A 111.1 . . ? Nd1 O9 H9B 110.4 . . ? H9A O9 H9B 108.9 . . ? Nd1 O10 H10A 109.3 . . ? Nd1 O10 H10B 109.9 . . ? H10A O10 H10B 109.1 . . ? H1WA O1W H1WB 109.3 . . ? O4 C1 C2 109.8(3) . . ? O4 C1 P1 106.6(3) . . ? C2 C1 P1 113.4(3) . . ? O4 C1 H1B 109.2 . . ? C2 C1 H1B 108.9 . . ? P1 C1 H1B 108.9 . . ? O5 C2 O6 124.8(4) . . ? O5 C2 C1 117.1(4) . . ? O6 C2 C1 118.1(3) . . ? O7 C3 O8 126.9(4) . . ? O7 C3 C3 117.0(5) . 3_656 ? O8 C3 C3 116.1(5) . 3_656 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.493 _refine_diff_density_min -1.046 _refine_diff_density_rms 0.149 # Attachment '670481.cif' data_0510a _database_code_depnum_ccdc_archive 'CCDC 670481' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H9 O11 P Sm' _chemical_formula_weight 402.42 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.2351(6) _cell_length_b 13.0550(10) _cell_length_c 10.1999(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.4270(10) _cell_angle_gamma 90.00 _cell_volume 947.51(13) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 3578 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 28.80 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.821 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 6.420 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5333 _exptl_absorpt_correction_T_max 0.8508 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Smart Apex II CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5035 _diffrn_reflns_av_R_equivalents 0.0208 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 26.00 _reflns_number_total 1856 _reflns_number_gt 1726 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0258P)^2^+1.3306P] 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 SHELXL _refine_ls_extinction_coef 0.0087(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1856 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0226 _refine_ls_R_factor_gt 0.0206 _refine_ls_wR_factor_ref 0.0523 _refine_ls_wR_factor_gt 0.0512 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _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 Sm1 Sm 0.83636(3) 0.094050(19) 0.71784(2) 0.01099(14) Uani 1 1 d . . . P1 P 1.21159(18) -0.04910(10) 0.93059(12) 0.0113(3) Uani 1 1 d . . . O1 O 1.3963(6) -0.0799(3) 0.8782(4) 0.0204(9) Uani 1 1 d . . . H1A H 1.4070 -0.0441 0.8139 0.031 Uiso 1 1 calc R . . O2 O 1.1283(5) 0.0484(3) 0.8682(3) 0.0166(8) Uani 1 1 d . . . O3 O 1.2535(5) -0.0537(3) 1.0795(3) 0.0181(8) Uani 1 1 d . . . O4 O 1.1554(5) -0.2475(3) 0.9261(3) 0.0162(8) Uani 1 1 d . . . H4A H 1.1341 -0.2601 1.0007 0.024 Uiso 1 1 calc R . . O5 O 0.9187(6) -0.0874(3) 0.6664(4) 0.0186(8) Uani 1 1 d . . . O6 O 1.0390(5) -0.2450(3) 0.6694(3) 0.0183(8) Uani 1 1 d . . . O7 O 0.6969(5) 0.0719(3) 0.4817(4) 0.0172(8) Uani 1 1 d . . . O8 O 0.4660(5) 0.0095(3) 0.3273(3) 0.0224(9) Uani 1 1 d . . . O9 O 1.1155(7) 0.1100(3) 0.6089(4) 0.0301(11) Uani 1 1 d . . . H9A H 1.1864 0.0593 0.6250 0.045 Uiso 1 1 d R . . H9B H 1.0827 0.1157 0.5262 0.045 Uiso 1 1 d R . . O10 O 0.5592(6) 0.2059(4) 0.7207(5) 0.0394(12) Uani 1 1 d . . . H10A H 0.4859 0.1772 0.7662 0.059 Uiso 1 1 d R . . H10B H 0.5939 0.2618 0.7554 0.059 Uiso 1 1 d R . . O1W O 0.3797(7) 0.2231(4) 0.9312(5) 0.0485(13) Uani 1 1 d . . . H1WA H 0.3931 0.1982 1.0081 0.073 Uiso 1 1 d R . . H1WB H 0.3887 0.2863 0.9366 0.073 Uiso 1 1 d R . . C1 C 1.0563(7) -0.1570(4) 0.8757(5) 0.0118(10) Uani 1 1 d . . . H1B H 0.9427 -0.1507 0.9149 0.014 Uiso 1 1 calc R . . C2 C 1.0000(7) -0.1638(4) 0.7256(5) 0.0140(11) Uani 1 1 d . . . C3 C 0.5468(7) 0.0242(4) 0.4451(5) 0.0150(11) 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 Sm1 0.01352(18) 0.01022(18) 0.00901(17) -0.00001(9) 0.00145(11) -0.00067(9) P1 0.0129(6) 0.0113(7) 0.0096(6) 0.0008(5) 0.0020(5) -0.0013(5) O1 0.020(2) 0.022(2) 0.022(2) 0.0079(16) 0.0117(17) 0.0039(16) O2 0.0184(19) 0.0105(19) 0.0197(19) -0.0010(15) 0.0006(15) 0.0009(15) O3 0.021(2) 0.023(2) 0.0102(18) 0.0005(15) 0.0010(15) -0.0065(16) O4 0.0252(19) 0.0103(18) 0.0137(18) 0.0025(14) 0.0053(15) 0.0010(15) O5 0.024(2) 0.013(2) 0.0164(19) -0.0001(14) -0.0018(16) 0.0048(15) O6 0.032(2) 0.0104(19) 0.0118(17) 0.0001(14) 0.0006(15) 0.0042(16) O7 0.0150(18) 0.021(2) 0.0157(18) -0.0021(15) 0.0027(15) -0.0042(15) O8 0.024(2) 0.034(2) 0.0090(17) -0.0004(16) 0.0014(15) -0.0124(18) O9 0.032(3) 0.040(3) 0.019(2) 0.0068(19) 0.0055(19) 0.015(2) O10 0.033(2) 0.031(3) 0.058(3) 0.012(2) 0.017(2) 0.008(2) O1W 0.034(3) 0.047(3) 0.065(4) -0.001(3) 0.008(2) 0.000(2) C1 0.013(2) 0.010(2) 0.013(2) 0.0014(19) 0.0035(18) -0.0003(19) C2 0.013(2) 0.013(3) 0.015(2) 0.000(2) 0.0006(19) -0.003(2) C3 0.015(3) 0.015(3) 0.015(3) 0.000(2) 0.003(2) 0.001(2) _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 Sm1 O3 2.336(3) 3_757 ? Sm1 O2 2.449(4) . ? Sm1 O7 2.454(4) . ? Sm1 O6 2.485(3) 2_756 ? Sm1 O5 2.521(3) . ? Sm1 O4 2.544(3) 2_756 ? Sm1 O8 2.542(4) 3_656 ? Sm1 O10 2.485(4) . ? Sm1 O9 2.484(5) . ? P1 O2 1.500(4) . ? P1 O3 1.495(4) . ? P1 O1 1.579(4) . ? P1 C1 1.826(5) . ? O1 H1A 0.8200 . ? O3 Sm1 2.336(3) 3_757 ? O4 C1 1.428(6) . ? O4 Sm1 2.544(3) 2_746 ? O4 H4A 0.8200 . ? O5 C2 1.256(6) . ? O6 C2 1.261(6) . ? O6 Sm1 2.485(3) 2_746 ? O7 C3 1.249(6) . ? O8 C3 1.252(6) . ? O8 Sm1 2.542(4) 3_656 ? O9 H9A 0.8354 . ? O9 H9B 0.8364 . ? O10 H10A 0.8525 . ? O10 H10B 0.8301 . ? O1W H1WA 0.8378 . ? O1W H1WB 0.8292 . ? C1 C2 1.514(6) . ? C1 H1B 0.9800 . ? C3 C3 1.546(9) 3_656 ? 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 Sm1 O2 74.78(12) 3_757 . ? O3 Sm1 O7 135.31(12) 3_757 . ? O2 Sm1 O7 137.81(12) . . ? O3 Sm1 O6 85.22(12) 3_757 2_756 ? O2 Sm1 O6 73.51(12) . 2_756 ? O7 Sm1 O6 127.17(12) . 2_756 ? O3 Sm1 O5 94.97(13) 3_757 . ? O2 Sm1 O5 72.08(12) . . ? O7 Sm1 O5 75.85(12) . . ? O6 Sm1 O5 144.22(13) 2_756 . ? O3 Sm1 O4 137.15(13) 3_757 2_756 ? O2 Sm1 O4 116.85(12) . 2_756 ? O7 Sm1 O4 65.04(12) . 2_756 ? O6 Sm1 O4 62.29(11) 2_756 2_756 ? O5 Sm1 O4 127.80(12) . 2_756 ? O3 Sm1 O8 70.88(12) 3_757 3_656 ? O2 Sm1 O8 126.91(12) . 3_656 ? O7 Sm1 O8 64.66(11) . 3_656 ? O6 Sm1 O8 139.63(13) 2_756 3_656 ? O5 Sm1 O8 71.98(13) . 3_656 ? O4 Sm1 O8 115.94(12) 2_756 3_656 ? O3 Sm1 O10 76.58(14) 3_757 . ? O2 Sm1 O10 137.90(14) . . ? O7 Sm1 O10 83.76(14) . . ? O6 Sm1 O10 73.95(15) 2_756 . ? O5 Sm1 O10 140.93(15) . . ? O4 Sm1 O10 68.41(13) 2_756 . ? O8 Sm1 O10 69.21(15) 3_656 . ? O3 Sm1 O9 142.52(14) 3_757 . ? O2 Sm1 O9 67.77(13) . . ? O7 Sm1 O9 78.11(13) . . ? O6 Sm1 O9 83.11(14) 2_756 . ? O5 Sm1 O9 75.13(14) . . ? O4 Sm1 O9 64.39(13) 2_756 . ? O8 Sm1 O9 134.93(14) 3_656 . ? O10 Sm1 O9 132.78(14) . . ? O2 P1 O3 117.2(2) . . ? O2 P1 O1 111.9(2) . . ? O3 P1 O1 107.8(2) . . ? O2 P1 C1 110.3(2) . . ? O3 P1 C1 106.3(2) . . ? O1 P1 C1 102.2(2) . . ? P1 O1 H1A 109.4 . . ? P1 O2 Sm1 135.0(2) . . ? P1 O3 Sm1 150.5(2) . 3_757 ? C1 O4 Sm1 121.9(3) . 2_746 ? C1 O4 H4A 109.2 . . ? Sm1 O4 H4A 113.8 2_746 . ? C2 O5 Sm1 138.9(3) . . ? C2 O6 Sm1 126.3(3) . 2_746 ? C3 O7 Sm1 122.2(3) . . ? C3 O8 Sm1 119.5(3) . 3_656 ? Sm1 O9 H9A 111.4 . . ? Sm1 O9 H9B 110.6 . . ? H9A O9 H9B 108.8 . . ? Sm1 O10 H10A 109.3 . . ? Sm1 O10 H10B 109.8 . . ? H10A O10 H10B 108.9 . . ? H1WA O1W H1WB 109.3 . . ? O4 C1 C2 109.9(4) . . ? O4 C1 P1 106.7(3) . . ? C2 C1 P1 113.2(3) . . ? O4 C1 H1B 109.3 . . ? C2 C1 H1B 108.9 . . ? P1 C1 H1B 108.8 . . ? O5 C2 O6 124.9(5) . . ? O5 C2 C1 117.2(4) . . ? O6 C2 C1 117.9(4) . . ? O7 C3 O8 126.4(5) . . ? O7 C3 C3 117.3(5) . 3_656 ? O8 C3 C3 116.3(6) . 3_656 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.636 _refine_diff_density_min -0.990 _refine_diff_density_rms 0.120 # Attachment '686602.cif' data_0320a _database_code_depnum_ccdc_archive 'CCDC 686602' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H9 Eu O11 P' _chemical_formula_weight 404.03 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' 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.2293(9) _cell_length_b 13.0429(16) _cell_length_c 10.1980(13) _cell_angle_alpha 90.00 _cell_angle_beta 100.541(2) _cell_angle_gamma 90.00 _cell_volume 945.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 4252 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 28.81 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.839 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 772 _exptl_absorpt_coefficient_mu 6.858 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3176 _exptl_absorpt_correction_T_max 0.7663 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Smart Apex II CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5600 _diffrn_reflns_av_R_equivalents 0.0197 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 27.73 _reflns_number_total 2215 _reflns_number_gt 2120 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0267P)^2^+3.3123P] 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 2215 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0255 _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_ref 0.0595 _refine_ls_wR_factor_gt 0.0589 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.002 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 0.83623(3) 0.093910(13) 0.717855(17) 0.00975(7) Uani 1 1 d . . . P1 P 1.21135(13) -0.04897(7) 0.93108(9) 0.00948(18) Uani 1 1 d . . . O1 O 1.3964(4) -0.0797(2) 0.8790(3) 0.0187(6) Uani 1 1 d . . . H1A H 1.4071 -0.0438 0.8148 0.028 Uiso 1 1 calc R . . O2 O 1.1276(4) 0.0487(2) 0.8680(3) 0.0154(6) Uani 1 1 d . . . O3 O 1.2529(4) -0.0533(2) 1.0801(3) 0.0166(6) Uani 1 1 d . . . O4 O 1.1562(4) -0.2477(2) 0.9264(3) 0.0145(5) Uani 1 1 d . . . H4A H 1.1354 -0.2607 1.0010 0.022 Uiso 1 1 calc R . . O5 O 0.9187(5) -0.0875(2) 0.6665(3) 0.0176(6) Uani 1 1 d . . . O6 O 1.0386(4) -0.2454(2) 0.6694(3) 0.0175(6) Uani 1 1 d . . . O7 O 0.6972(4) 0.0714(2) 0.4820(3) 0.0162(6) Uani 1 1 d . . . O8 O 0.4665(4) 0.0090(2) 0.3275(3) 0.0206(6) Uani 1 1 d . . . O9 O 1.1142(5) 0.1090(3) 0.6087(3) 0.0263(7) Uani 1 1 d . . . H9A H 1.1850 0.0583 0.6249 0.039 Uiso 1 1 d R . . H9B H 1.0813 0.1147 0.5261 0.039 Uiso 1 1 d R . . O10 O 0.5602(5) 0.2053(3) 0.7203(4) 0.0376(9) Uani 1 1 d . . . H10A H 0.4869 0.1766 0.7658 0.056 Uiso 1 1 d R . . H10B H 0.5949 0.2612 0.7550 0.056 Uiso 1 1 d R . . O1W O 0.3798(6) 0.2239(3) 0.9308(5) 0.0483(10) Uani 1 1 d . . . H1WA H 0.3933 0.1990 1.0076 0.072 Uiso 1 1 d R . . H1WB H 0.3888 0.2872 0.9362 0.072 Uiso 1 1 d R . . C1 C 1.0560(5) -0.1573(3) 0.8765(4) 0.0105(7) Uani 1 1 d . . . H1B H 0.9423 -0.1513 0.9156 0.013 Uiso 1 1 calc R . . C2 C 1.0004(5) -0.1638(3) 0.7260(4) 0.0114(7) Uani 1 1 d . . . C3 C 0.5476(5) 0.0244(3) 0.4448(4) 0.0129(7) 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 Eu1 0.00949(11) 0.01061(11) 0.00831(11) 0.00006(6) -0.00057(7) -0.00069(6) P1 0.0083(4) 0.0114(4) 0.0082(4) -0.0001(3) 0.0001(3) -0.0014(3) O1 0.0140(14) 0.0225(14) 0.0218(15) 0.0065(11) 0.0089(12) 0.0022(12) O2 0.0149(14) 0.0114(12) 0.0180(14) 0.0012(10) -0.0022(11) 0.0005(11) O3 0.0161(14) 0.0240(14) 0.0091(12) -0.0006(11) 0.0007(11) -0.0054(12) O4 0.0220(15) 0.0111(12) 0.0095(12) 0.0024(9) 0.0001(11) 0.0009(11) O5 0.0217(16) 0.0140(13) 0.0143(14) 0.0004(10) -0.0044(12) 0.0024(11) O6 0.0266(16) 0.0130(13) 0.0118(13) -0.0019(10) 0.0003(12) 0.0030(11) O7 0.0141(14) 0.0207(13) 0.0127(13) -0.0017(11) -0.0003(11) -0.0051(11) O8 0.0173(15) 0.0335(16) 0.0096(13) 0.0006(11) -0.0010(11) -0.0113(13) O9 0.0257(17) 0.0387(18) 0.0147(15) 0.0076(13) 0.0046(13) 0.0139(15) O10 0.030(2) 0.0315(18) 0.055(2) 0.0129(17) 0.0188(18) 0.0108(16) O1W 0.029(2) 0.047(2) 0.068(3) 0.001(2) 0.006(2) 0.0008(19) C1 0.0105(17) 0.0115(16) 0.0092(16) -0.0004(13) 0.0008(13) -0.0020(13) C2 0.0083(16) 0.0127(16) 0.0118(17) -0.0011(13) -0.0016(14) -0.0034(14) C3 0.0124(18) 0.0153(17) 0.0105(17) -0.0006(13) 0.0007(14) 0.0005(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 Eu1 O3 2.330(3) 3_757 ? Eu1 O2 2.439(3) . ? Eu1 O7 2.449(3) . ? Eu1 O10 2.472(3) . ? Eu1 O9 2.476(3) . ? Eu1 O6 2.480(3) 2_756 ? Eu1 O5 2.518(3) . ? Eu1 O8 2.537(3) 3_656 ? Eu1 O4 2.542(3) 2_756 ? P1 O3 1.495(3) . ? P1 O2 1.503(3) . ? P1 O1 1.579(3) . ? P1 C1 1.827(4) . ? O1 H1A 0.8200 . ? O3 Eu1 2.330(3) 3_757 ? O4 C1 1.428(4) . ? O4 Eu1 2.542(3) 2_746 ? O4 H4A 0.8200 . ? O5 C2 1.256(4) . ? O6 C2 1.265(4) . ? O6 Eu1 2.480(3) 2_746 ? O7 C3 1.241(5) . ? O8 C3 1.249(5) . ? O8 Eu1 2.537(3) 3_656 ? O9 H9A 0.8345 . ? O9 H9B 0.8357 . ? O10 H10A 0.8526 . ? O10 H10B 0.8292 . ? O1W H1WA 0.8374 . ? O1W H1WB 0.8284 . ? C1 C2 1.516(5) . ? C1 H1B 0.9800 . ? C3 C3 1.559(7) 3_656 ? 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 O2 74.73(10) 3_757 . ? O3 Eu1 O7 135.34(10) 3_757 . ? O2 Eu1 O7 137.73(10) . . ? O3 Eu1 O10 76.72(11) 3_757 . ? O2 Eu1 O10 137.88(12) . . ? O7 Eu1 O10 83.85(12) . . ? O3 Eu1 O9 142.57(11) 3_757 . ? O2 Eu1 O9 67.85(10) . . ? O7 Eu1 O9 77.83(10) . . ? O10 Eu1 O9 132.87(11) . . ? O3 Eu1 O6 85.33(9) 3_757 2_756 ? O2 Eu1 O6 73.34(9) . 2_756 ? O7 Eu1 O6 127.28(9) . 2_756 ? O10 Eu1 O6 74.08(12) . 2_756 ? O9 Eu1 O6 83.32(11) . 2_756 ? O3 Eu1 O5 94.87(10) 3_757 . ? O2 Eu1 O5 72.15(9) . . ? O7 Eu1 O5 75.73(10) . . ? O10 Eu1 O5 140.93(12) . . ? O9 Eu1 O5 74.87(11) . . ? O6 Eu1 O5 144.10(10) 2_756 . ? O3 Eu1 O8 70.85(9) 3_757 3_656 ? O2 Eu1 O8 127.13(10) . 3_656 ? O7 Eu1 O8 64.68(9) . 3_656 ? O10 Eu1 O8 69.01(12) . 3_656 ? O9 Eu1 O8 134.76(11) . 3_656 ? O6 Eu1 O8 139.56(10) 2_756 3_656 ? O5 Eu1 O8 72.18(11) . 3_656 ? O3 Eu1 O4 137.31(9) 3_757 2_756 ? O2 Eu1 O4 116.89(9) . 2_756 ? O7 Eu1 O4 64.99(9) . 2_756 ? O10 Eu1 O4 68.35(11) . 2_756 ? O9 Eu1 O4 64.54(10) . 2_756 ? O6 Eu1 O4 62.43(9) 2_756 2_756 ? O5 Eu1 O4 127.73(9) . 2_756 ? O8 Eu1 O4 115.70(10) 3_656 2_756 ? O3 P1 O2 117.22(17) . . ? O3 P1 O1 107.89(17) . . ? O2 P1 O1 111.77(16) . . ? O3 P1 C1 106.14(16) . . ? O2 P1 C1 110.37(17) . . ? O1 P1 C1 102.27(17) . . ? P1 O1 H1A 109.5 . . ? P1 O2 Eu1 135.01(16) . . ? P1 O3 Eu1 150.57(18) . 3_757 ? C1 O4 Eu1 121.9(2) . 2_746 ? C1 O4 H4A 109.5 . . ? Eu1 O4 H4A 113.4 2_746 . ? C2 O5 Eu1 138.8(2) . . ? C2 O6 Eu1 126.2(2) . 2_746 ? C3 O7 Eu1 122.5(2) . . ? C3 O8 Eu1 119.9(2) . 3_656 ? Eu1 O9 H9A 111.5 . . ? Eu1 O9 H9B 110.9 . . ? H9A O9 H9B 108.7 . . ? Eu1 O10 H10A 109.3 . . ? Eu1 O10 H10B 109.8 . . ? H10A O10 H10B 108.9 . . ? H1WA O1W H1WB 109.3 . . ? O4 C1 C2 109.7(3) . . ? O4 C1 P1 106.7(2) . . ? C2 C1 P1 112.7(2) . . ? O4 C1 H1B 109.2 . . ? C2 C1 H1B 109.2 . . ? P1 C1 H1B 109.2 . . ? O5 C2 O6 124.7(3) . . ? O5 C2 C1 117.3(3) . . ? O6 C2 C1 118.0(3) . . ? O7 C3 O8 127.1(3) . . ? O7 C3 C3 117.1(4) . 3_656 ? O8 C3 C3 115.8(4) . 3_656 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.73 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.967 _refine_diff_density_min -1.978 _refine_diff_density_rms 0.158