# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_publication_text _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H6 Er2 O10.50 P3' _chemical_formula_weight 637.51 _chemical_absolute_configuration unk 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M I2(1)3 _symmetry_space_group_name_Hall 'I 2b 2c 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-x+1/2, y+1, -z+1' 'x+1, -y+1, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1, -x+1, -y+1/2' '-z+1, -x+1/2, y+1' '-z+1/2, x+1, -y+1' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1, -x+1' 'y+1, -z+1, -x+1/2' '-y+1, -z+1/2, x+1' _cell_length_a 13.4484(2) _cell_length_b 13.4484(2) _cell_length_c 13.4484(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2432.27(6) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9908 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 39.85 _exptl_crystal_description cubic _exptl_crystal_colour pink _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2312 _exptl_absorpt_coefficient_mu 14.146 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1850 _exptl_absorpt_correction_T_max 0.2816 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 20021 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0260 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 40.17 _reflns_number_total 2564 _reflns_number_gt 2453 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0300P)^2^+33.9595P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(2) _refine_ls_number_reflns 2564 _refine_ls_number_parameters 68 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0844 _refine_ls_wR_factor_gt 0.0834 _refine_ls_goodness_of_fit_ref 1.200 _refine_ls_restrained_S_all 1.200 _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 Er1 Er 0.568716(15) 0.431284(15) 0.931284(15) 0.01046(6) Uani 1 3 d S . . Er2 Er 0.715817(19) 0.284183(19) 0.784183(19) 0.01842(8) Uani 1 3 d S . . P1 P 0.64158(11) 0.19555(11) 1.02499(10) 0.0152(2) Uani 1 1 d . . . O1 O 0.6413(3) 0.2769(3) 0.9438(3) 0.0182(7) Uani 1 1 d . . . O2 O 0.8429(4) 0.2364(7) 0.8715(4) 0.048(2) Uani 1 1 d . . . O3 O 0.4835(4) 0.5524(3) 0.8706(3) 0.0240(9) Uani 1 1 d . . . O4A O 0.7326(13) 0.0238(10) 0.9693(16) 0.057(6) Uani 0.259(10) 1 d P . 1 C2A C 0.7326(13) 0.0238(10) 0.9693(16) 0.057(6) Uani 0.259(10) 1 d P . 1 O4B O 0.7632(12) 0.1083(12) 1.1310(11) 0.038(4) Uani 0.241(10) 1 d P . 2 C2B C 0.7632(12) 0.1083(12) 1.1310(11) 0.038(4) Uani 0.241(10) 1 d P . 2 C1 C 0.7500 0.1205(8) 1.0000 0.043(3) Uani 1 2 d S . . 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 Er1 0.01046(6) 0.01046(6) 0.01046(6) 0.00146(6) -0.00146(6) -0.00146(6) Er2 0.01842(8) 0.01842(8) 0.01842(8) 0.00050(8) -0.00050(8) -0.00050(8) P1 0.0136(5) 0.0161(5) 0.0159(5) 0.0049(4) -0.0045(4) -0.0068(4) O1 0.0118(13) 0.0195(16) 0.0234(18) 0.0103(14) -0.0014(12) 0.0032(12) O2 0.031(3) 0.099(6) 0.0153(19) 0.007(3) 0.0042(18) 0.041(3) O3 0.033(2) 0.0176(18) 0.0217(19) 0.0088(14) 0.0079(16) 0.0124(16) O4A 0.044(10) 0.024(6) 0.104(19) -0.027(8) 0.006(9) 0.007(5) C2A 0.044(10) 0.024(6) 0.104(19) -0.027(8) 0.006(9) 0.007(5) O4B 0.038(8) 0.046(8) 0.032(7) 0.003(6) -0.007(5) 0.004(6) C2B 0.038(8) 0.046(8) 0.032(7) 0.003(6) -0.007(5) 0.004(6) C1 0.019(4) 0.019(4) 0.093(11) 0.000 -0.016(5) 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 Er1 O3 2.152(4) 7_665 ? Er1 O3 2.152(4) . ? Er1 O3 2.152(4) 10_646 ? Er1 O1 2.301(4) . ? Er1 O1 2.301(4) 7_665 ? Er1 O1 2.301(4) 10_646 ? Er1 Er2 3.4265(6) . ? Er2 O2 2.171(5) 7_665 ? Er2 O2 2.171(5) 10_646 ? Er2 O2 2.171(5) . ? Er2 O1 2.371(4) 10_646 ? Er2 O1 2.371(4) 7_665 ? Er2 O1 2.371(4) . ? Er2 C2B 2.641(17) 17_445 ? Er2 O4B 2.641(17) 17_445 ? Er2 C2B 2.641(17) 24_564 ? Er2 O4B 2.641(17) 24_564 ? Er2 O4B 2.641(17) 15_646 ? Er2 C2B 2.641(17) 15_646 ? P1 O3 1.498(4) 23_456 ? P1 O2 1.511(6) 15_646 ? P1 O1 1.545(4) . ? P1 C1 1.805(6) . ? O2 P1 1.511(6) 15_646 ? O3 P1 1.498(4) 20_645 ? O4A C2A 0.95(4) 15_646 ? O4A O4A 0.95(4) 15_646 ? O4A C1 1.384(16) . ? O4B C1 1.779(15) . ? O4B Er2 2.641(17) 15_646 ? C1 C2A 1.384(16) 15_646 ? C1 O4A 1.384(16) 15_646 ? C1 C2B 1.779(15) 15_646 ? C1 O4B 1.779(15) 15_646 ? C1 P1 1.805(6) 15_646 ? 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 Er1 O3 94.91(16) 7_665 . ? O3 Er1 O3 94.91(16) 7_665 10_646 ? O3 Er1 O3 94.91(16) . 10_646 ? O3 Er1 O1 105.35(17) 7_665 . ? O3 Er1 O1 159.50(18) . . ? O3 Er1 O1 86.54(16) 10_646 . ? O3 Er1 O1 159.50(18) 7_665 7_665 ? O3 Er1 O1 86.54(16) . 7_665 ? O3 Er1 O1 105.35(17) 10_646 7_665 ? O1 Er1 O1 73.40(16) . 7_665 ? O3 Er1 O1 86.54(17) 7_665 10_646 ? O3 Er1 O1 105.35(17) . 10_646 ? O3 Er1 O1 159.50(18) 10_646 10_646 ? O1 Er1 O1 73.40(16) . 10_646 ? O1 Er1 O1 73.40(16) 7_665 10_646 ? O3 Er1 Er2 121.71(12) 7_665 . ? O3 Er1 Er2 121.71(12) . . ? O3 Er1 Er2 121.71(12) 10_646 . ? O1 Er1 Er2 43.64(10) . . ? O1 Er1 Er2 43.64(10) 7_665 . ? O1 Er1 Er2 43.64(10) 10_646 . ? O2 Er2 O2 110.68(15) 7_665 10_646 ? O2 Er2 O2 110.68(15) 7_665 . ? O2 Er2 O2 110.67(15) 10_646 . ? O2 Er2 O1 149.35(17) 7_665 10_646 ? O2 Er2 O1 80.26(16) 10_646 10_646 ? O2 Er2 O1 90.4(3) . 10_646 ? O2 Er2 O1 80.26(16) 7_665 7_665 ? O2 Er2 O1 90.4(3) 10_646 7_665 ? O2 Er2 O1 149.35(17) . 7_665 ? O1 Er2 O1 70.88(15) 10_646 7_665 ? O2 Er2 O1 90.4(3) 7_665 . ? O2 Er2 O1 149.35(17) 10_646 . ? O2 Er2 O1 80.26(16) . . ? O1 Er2 O1 70.88(15) 10_646 . ? O1 Er2 O1 70.88(15) 7_665 . ? O2 Er2 C2B 54.4(4) 7_665 17_445 ? O2 Er2 C2B 58.7(4) 10_646 17_445 ? O2 Er2 C2B 142.5(4) . 17_445 ? O1 Er2 C2B 119.6(4) 10_646 17_445 ? O1 Er2 C2B 67.5(4) 7_665 17_445 ? O1 Er2 C2B 128.6(3) . 17_445 ? O2 Er2 O4B 54.4(4) 7_665 17_445 ? O2 Er2 O4B 58.7(4) 10_646 17_445 ? O2 Er2 O4B 142.5(4) . 17_445 ? O1 Er2 O4B 119.6(4) 10_646 17_445 ? O1 Er2 O4B 67.5(4) 7_665 17_445 ? O1 Er2 O4B 128.6(3) . 17_445 ? C2B Er2 O4B 0.0(9) 17_445 17_445 ? O2 Er2 C2B 142.5(4) 7_665 24_564 ? O2 Er2 C2B 54.4(4) 10_646 24_564 ? O2 Er2 C2B 58.7(4) . 24_564 ? O1 Er2 C2B 67.5(4) 10_646 24_564 ? O1 Er2 C2B 128.6(3) 7_665 24_564 ? O1 Er2 C2B 119.6(4) . 24_564 ? C2B Er2 C2B 109.7(4) 17_445 24_564 ? O4B Er2 C2B 109.7(4) 17_445 24_564 ? O2 Er2 O4B 142.5(4) 7_665 24_564 ? O2 Er2 O4B 54.4(4) 10_646 24_564 ? O2 Er2 O4B 58.7(4) . 24_564 ? O1 Er2 O4B 67.5(4) 10_646 24_564 ? O1 Er2 O4B 128.6(3) 7_665 24_564 ? O1 Er2 O4B 119.6(4) . 24_564 ? C2B Er2 O4B 109.7(4) 17_445 24_564 ? O4B Er2 O4B 109.7(4) 17_445 24_564 ? C2B Er2 O4B 0.0(8) 24_564 24_564 ? O2 Er2 O4B 58.7(4) 7_665 15_646 ? O2 Er2 O4B 142.5(4) 10_646 15_646 ? O2 Er2 O4B 54.4(4) . 15_646 ? O1 Er2 O4B 128.6(3) 10_646 15_646 ? O1 Er2 O4B 119.6(4) 7_665 15_646 ? O1 Er2 O4B 67.5(4) . 15_646 ? C2B Er2 O4B 109.7(4) 17_445 15_646 ? O4B Er2 O4B 109.7(4) 17_445 15_646 ? C2B Er2 O4B 109.7(4) 24_564 15_646 ? O4B Er2 O4B 109.7(4) 24_564 15_646 ? O2 Er2 C2B 58.7(4) 7_665 15_646 ? O2 Er2 C2B 142.5(4) 10_646 15_646 ? O2 Er2 C2B 54.4(4) . 15_646 ? O1 Er2 C2B 128.6(3) 10_646 15_646 ? O1 Er2 C2B 119.6(4) 7_665 15_646 ? O1 Er2 C2B 67.5(4) . 15_646 ? C2B Er2 C2B 109.7(4) 17_445 15_646 ? O4B Er2 C2B 109.7(4) 17_445 15_646 ? C2B Er2 C2B 109.7(4) 24_564 15_646 ? O4B Er2 C2B 109.7(4) 24_564 15_646 ? O4B Er2 C2B 0.0(3) 15_646 15_646 ? O3 P1 O2 113.4(3) 23_456 15_646 ? O3 P1 O1 111.4(2) 23_456 . ? O2 P1 O1 113.2(4) 15_646 . ? O3 P1 C1 107.5(3) 23_456 . ? O2 P1 C1 105.3(3) 15_646 . ? O1 P1 C1 105.5(3) . . ? P1 O1 Er1 133.8(3) . . ? P1 O1 Er2 131.9(2) . . ? Er1 O1 Er2 94.33(14) . . ? P1 O2 Er2 135.6(3) 15_646 . ? P1 O3 Er1 150.6(3) 20_645 . ? C2A O4A O4A 0.0(17) 15_646 15_646 ? C2A O4A C1 69.9(8) 15_646 . ? O4A O4A C1 69.9(8) 15_646 . ? C1 O4B Er2 110.8(8) . 15_646 ? C2A C1 O4A 0.0(4) 15_646 15_646 ? C2A C1 O4A 40.2(17) 15_646 . ? O4A C1 O4A 40.2(17) 15_646 . ? C2A C1 O4B 66.5(11) 15_646 . ? O4A C1 O4B 66.5(11) 15_646 . ? O4A C1 O4B 103.1(12) . . ? C2A C1 C2B 103.1(12) 15_646 15_646 ? O4A C1 C2B 103.1(12) 15_646 15_646 ? O4A C1 C2B 66.5(11) . 15_646 ? O4B C1 C2B 169.4(13) . 15_646 ? C2A C1 O4B 103.1(12) 15_646 15_646 ? O4A C1 O4B 103.1(12) 15_646 15_646 ? O4A C1 O4B 66.5(11) . 15_646 ? O4B C1 O4B 169.4(13) . 15_646 ? C2B C1 O4B 0.0(15) 15_646 15_646 ? C2A C1 P1 116.4(7) 15_646 15_646 ? O4A C1 P1 116.4(7) 15_646 15_646 ? O4A C1 P1 127.3(8) . 15_646 ? O4B C1 P1 98.9(6) . 15_646 ? C2B C1 P1 87.0(6) 15_646 15_646 ? O4B C1 P1 87.0(6) 15_646 15_646 ? C2A C1 P1 127.3(8) 15_646 . ? O4A C1 P1 127.3(8) 15_646 . ? O4A C1 P1 116.4(7) . . ? O4B C1 P1 87.0(6) . . ? C2B C1 P1 98.9(6) 15_646 . ? O4B C1 P1 98.9(6) 15_646 . ? P1 C1 P1 112.0(6) 15_646 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 40.17 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.767 _refine_diff_density_min -4.054 _refine_diff_density_rms 0.288 _database_code_depnum_ccdc_archive 'CCDC 927686' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_publication_text _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C H2.33 O6.67 P2 Y1.33' _chemical_formula_weight 301.52 _chemical_absolute_configuration unk 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M I2(1)3 _symmetry_space_group_name_Hall 'I 2b 2c 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-x+1/2, y+1, -z+1' 'x+1, -y+1, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1, -x+1, -y+1/2' '-z+1, -x+1/2, y+1' '-z+1/2, x+1, -y+1' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1, -x+1' 'y+1, -z+1, -x+1/2' '-y+1, -z+1/2, x+1' _cell_length_a 13.5171(2) _cell_length_b 13.5171(2) _cell_length_c 13.5171(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2469.74(6) _cell_formula_units_Z 12 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 5193 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 32.16 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1724 _exptl_absorpt_coefficient_mu 9.774 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3867 _exptl_absorpt_correction_T_max 0.4415 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11402 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.69 _diffrn_reflns_theta_max 32.43 _reflns_number_total 1479 _reflns_number_gt 1301 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0775P)^2^+4.8505P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.007(14) _refine_ls_number_reflns 1479 _refine_ls_number_parameters 52 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1264 _refine_ls_wR_factor_gt 0.1214 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _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 Y1 Y 0.18277(3) 0.68277(3) 0.81723(3) 0.01517(18) Uani 1 3 d S . . Y2 Y 0.03178(4) 0.53178(4) 0.96822(4) 0.0232(2) Uani 1 3 d S . . P1 P 0.10719(10) 0.77187(10) 1.05248(10) 0.0186(3) Uani 1 1 d . . . O1 O 0.1127(3) 0.6910(3) 0.9727(3) 0.0235(8) Uani 1 1 d . . . O2 O -0.0963(3) 0.6278(3) 1.0062(5) 0.0377(11) Uani 1 1 d . . . O3 O 0.1243(3) 0.8100(4) 0.7362(4) 0.0349(11) Uani 1 1 d . . . O4 O -0.0701(5) 0.4299(5) 1.0701(5) 0.058(3) Uani 1 3 d S . . H4A H -0.0488 0.3836 1.1113 0.070 Uiso 0.33 1 d PR . . H4B H -0.0601 0.4890 1.0920 0.070 Uiso 0.33 1 d PR . . C1 C 0.0000 0.7500 1.1137(6) 0.0268(16) Uani 1 2 d S . . H1 H 0.0000 0.7500 1.1840 0.032 Uiso 1 2 calc SR . . 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 Y1 0.01517(18) 0.01517(18) 0.01517(18) -0.00113(16) -0.00113(16) 0.00113(16) Y2 0.0232(2) 0.0232(2) 0.0232(2) -0.00149(19) -0.00149(19) 0.00149(19) P1 0.0177(6) 0.0213(6) 0.0168(6) -0.0041(4) -0.0034(5) 0.0056(5) O1 0.0192(16) 0.0293(19) 0.0220(17) -0.0134(16) 0.0016(14) 0.0006(15) O2 0.030(2) 0.027(2) 0.056(3) -0.006(2) 0.013(2) 0.0031(17) O3 0.033(2) 0.039(2) 0.032(2) 0.012(2) 0.0072(18) 0.020(2) O4 0.058(3) 0.058(3) 0.058(3) 0.009(3) 0.009(3) -0.009(3) C1 0.011(3) 0.045(5) 0.024(3) 0.000 0.000 0.010(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 Y1 O3 2.186(5) . ? Y1 O3 2.186(5) 11_466 ? Y1 O3 2.186(5) 8_656 ? Y1 O1 2.308(4) . ? Y1 O1 2.308(4) 11_466 ? Y1 O1 2.308(4) 8_656 ? Y1 Y2 3.5351(13) . ? Y2 O2 2.224(5) . ? Y2 O2 2.224(5) 11_466 ? Y2 O2 2.224(5) 8_656 ? Y2 O4 2.386(12) . ? Y2 O1 2.415(4) 8_656 ? Y2 O1 2.415(4) . ? Y2 O1 2.415(4) 11_466 ? Y2 H4B 2.1629 . ? P1 O3 1.486(4) 24_565 ? P1 O2 1.500(5) 14_464 ? P1 O1 1.537(4) . ? P1 C1 1.694(5) . ? O2 P1 1.500(5) 14_464 ? O3 P1 1.486(4) 18_356 ? O4 H4A 0.8853 . ? O4 H4B 0.8628 . ? C1 P1 1.694(4) 14_464 ? C1 H1 0.9500 . ? 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 Y1 O3 94.08(16) . 11_466 ? O3 Y1 O3 94.08(16) . 8_656 ? O3 Y1 O3 94.08(16) 11_466 8_656 ? O3 Y1 O1 105.66(16) . . ? O3 Y1 O1 88.25(17) 11_466 . ? O3 Y1 O1 159.91(18) 8_656 . ? O3 Y1 O1 159.91(18) . 11_466 ? O3 Y1 O1 105.66(16) 11_466 11_466 ? O3 Y1 O1 88.25(17) 8_656 11_466 ? O1 Y1 O1 71.95(17) . 11_466 ? O3 Y1 O1 88.25(17) . 8_656 ? O3 Y1 O1 159.91(18) 11_466 8_656 ? O3 Y1 O1 105.66(16) 8_656 8_656 ? O1 Y1 O1 71.95(17) . 8_656 ? O1 Y1 O1 71.95(17) 11_466 8_656 ? O3 Y1 Y2 122.32(12) . . ? O3 Y1 Y2 122.32(12) 11_466 . ? O3 Y1 Y2 122.32(12) 8_656 . ? O1 Y1 Y2 42.71(11) . . ? O1 Y1 Y2 42.71(11) 11_466 . ? O1 Y1 Y2 42.71(11) 8_656 . ? O2 Y2 O2 114.17(10) . 11_466 ? O2 Y2 O2 114.17(10) . 8_656 ? O2 Y2 O2 114.17(10) 11_466 8_656 ? O2 Y2 O4 75.77(13) . . ? O2 Y2 O4 75.77(13) 11_466 . ? O2 Y2 O4 75.77(13) 8_656 . ? O2 Y2 O1 85.52(18) . 8_656 ? O2 Y2 O1 144.39(16) 11_466 8_656 ? O2 Y2 O1 80.01(15) 8_656 8_656 ? O4 Y2 O1 139.60(9) . 8_656 ? O2 Y2 O1 80.01(15) . . ? O2 Y2 O1 85.52(18) 11_466 . ? O2 Y2 O1 144.39(16) 8_656 . ? O4 Y2 O1 139.60(9) . . ? O1 Y2 O1 68.30(14) 8_656 . ? O2 Y2 O1 144.39(16) . 11_466 ? O2 Y2 O1 80.01(15) 11_466 11_466 ? O2 Y2 O1 85.52(18) 8_656 11_466 ? O4 Y2 O1 139.60(9) . 11_466 ? O1 Y2 O1 68.30(14) 8_656 11_466 ? O1 Y2 O1 68.30(14) . 11_466 ? O2 Y2 Y1 104.23(13) . . ? O2 Y2 Y1 104.23(13) 11_466 . ? O2 Y2 Y1 104.23(13) 8_656 . ? O4 Y2 Y1 180.00(14) . . ? O1 Y2 Y1 40.40(9) 8_656 . ? O1 Y2 Y1 40.40(9) . . ? O1 Y2 Y1 40.40(9) 11_466 . ? O2 Y2 H4B 62.0 . . ? O2 Y2 H4B 70.8 11_466 . ? O2 Y2 H4B 96.4 8_656 . ? O4 Y2 H4B 21.1 . . ? O1 Y2 H4B 142.8 8_656 . ? O1 Y2 H4B 118.6 . . ? O1 Y2 H4B 148.8 11_466 . ? Y1 Y2 H4B 158.9 . . ? O3 P1 O2 114.4(3) 24_565 14_464 ? O3 P1 O1 111.7(2) 24_565 . ? O2 P1 O1 110.8(3) 14_464 . ? O3 P1 C1 108.2(3) 24_565 . ? O2 P1 C1 106.1(2) 14_464 . ? O1 P1 C1 105.1(2) . . ? P1 O1 Y1 133.9(3) . . ? P1 O1 Y2 129.0(2) . . ? Y1 O1 Y2 96.89(14) . . ? P1 O2 Y2 134.5(3) 14_464 . ? P1 O3 Y1 149.9(3) 18_356 . ? Y2 O4 H4A 125.7 . . ? Y2 O4 H4B 64.7 . . ? H4A O4 H4B 112.8 . . ? P1 C1 P1 121.6(5) 14_464 . ? P1 C1 H1 119.2 14_464 . ? P1 C1 H1 119.2 . . ? 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 Y1 Y2 O2 -22.7(2) . . . . ? O3 Y1 Y2 O2 97.3(2) 11_466 . . . ? O3 Y1 Y2 O2 -142.7(2) 8_656 . . . ? O1 Y1 Y2 O2 55.0(2) . . . . ? O1 Y1 Y2 O2 175.0(2) 11_466 . . . ? O1 Y1 Y2 O2 -65.0(2) 8_656 . . . ? O3 Y1 Y2 O2 -142.7(2) . . . 11_466 ? O3 Y1 Y2 O2 -22.7(2) 11_466 . . 11_466 ? O3 Y1 Y2 O2 97.3(2) 8_656 . . 11_466 ? O1 Y1 Y2 O2 -65.0(2) . . . 11_466 ? O1 Y1 Y2 O2 55.0(2) 11_466 . . 11_466 ? O1 Y1 Y2 O2 175.0(2) 8_656 . . 11_466 ? O3 Y1 Y2 O2 97.3(2) . . . 8_656 ? O3 Y1 Y2 O2 -142.7(2) 11_466 . . 8_656 ? O3 Y1 Y2 O2 -22.7(2) 8_656 . . 8_656 ? O1 Y1 Y2 O2 175.0(2) . . . 8_656 ? O1 Y1 Y2 O2 -65.0(2) 11_466 . . 8_656 ? O1 Y1 Y2 O2 55.0(2) 8_656 . . 8_656 ? O3 Y1 Y2 O4 23(100) . . . . ? O3 Y1 Y2 O4 143(100) 11_466 . . . ? O3 Y1 Y2 O4 -97(100) 8_656 . . . ? O1 Y1 Y2 O4 100(100) . . . . ? O1 Y1 Y2 O4 -140(100) 11_466 . . . ? O1 Y1 Y2 O4 -20(100) 8_656 . . . ? O3 Y1 Y2 O1 42.4(2) . . . 8_656 ? O3 Y1 Y2 O1 162.4(2) 11_466 . . 8_656 ? O3 Y1 Y2 O1 -77.6(2) 8_656 . . 8_656 ? O1 Y1 Y2 O1 120.0 . . . 8_656 ? O1 Y1 Y2 O1 -120.0 11_466 . . 8_656 ? O3 Y1 Y2 O1 -77.6(2) . . . . ? O3 Y1 Y2 O1 42.4(2) 11_466 . . . ? O3 Y1 Y2 O1 162.4(2) 8_656 . . . ? O1 Y1 Y2 O1 120.0 11_466 . . . ? O1 Y1 Y2 O1 -120.0 8_656 . . . ? O3 Y1 Y2 O1 162.4(2) . . . 11_466 ? O3 Y1 Y2 O1 -77.6(2) 11_466 . . 11_466 ? O3 Y1 Y2 O1 42.4(2) 8_656 . . 11_466 ? O1 Y1 Y2 O1 -120.0 . . . 11_466 ? O1 Y1 Y2 O1 120.0 8_656 . . 11_466 ? O3 P1 O1 Y1 -92.2(4) 24_565 . . . ? O2 P1 O1 Y1 36.5(4) 14_464 . . . ? C1 P1 O1 Y1 150.7(3) . . . . ? O3 P1 O1 Y2 94.7(4) 24_565 . . . ? O2 P1 O1 Y2 -136.5(3) 14_464 . . . ? C1 P1 O1 Y2 -22.3(4) . . . . ? O3 Y1 O1 P1 -53.6(4) . . . . ? O3 Y1 O1 P1 40.2(3) 11_466 . . . ? O3 Y1 O1 P1 137.3(4) 8_656 . . . ? O1 Y1 O1 P1 147.3(4) 11_466 . . . ? O1 Y1 O1 P1 -136.4(4) 8_656 . . . ? Y2 Y1 O1 P1 -174.5(4) . . . . ? O3 Y1 O1 Y2 120.99(19) . . . . ? O3 Y1 O1 Y2 -145.26(17) 11_466 . . . ? O3 Y1 O1 Y2 -48.1(5) 8_656 . . . ? O1 Y1 O1 Y2 -38.16(5) 11_466 . . . ? O1 Y1 O1 Y2 38.16(5) 8_656 . . . ? O2 Y2 O1 P1 48.6(3) . . . . ? O2 Y2 O1 P1 -66.9(3) 11_466 . . . ? O2 Y2 O1 P1 166.5(3) 8_656 . . . ? O4 Y2 O1 P1 -5.1(4) . . . . ? O1 Y2 O1 P1 137.8(4) 8_656 . . . ? O1 Y2 O1 P1 -147.9(4) 11_466 . . . ? Y1 Y2 O1 P1 174.9(4) . . . . ? O2 Y2 O1 Y1 -126.3(2) . . . . ? O2 Y2 O1 Y1 118.18(17) 11_466 . . . ? O2 Y2 O1 Y1 -8.4(4) 8_656 . . . ? O4 Y2 O1 Y1 180.0 . . . . ? O1 Y2 O1 Y1 -37.17(4) 8_656 . . . ? O1 Y2 O1 Y1 37.17(4) 11_466 . . . ? O2 Y2 O2 P1 58.0(7) 11_466 . . 14_464 ? O2 Y2 O2 P1 -168.1(4) 8_656 . . 14_464 ? O4 Y2 O2 P1 125.0(5) . . . 14_464 ? O1 Y2 O2 P1 -91.1(5) 8_656 . . 14_464 ? O1 Y2 O2 P1 -22.4(5) . . . 14_464 ? O1 Y2 O2 P1 -49.4(7) 11_466 . . 14_464 ? Y1 Y2 O2 P1 -55.0(5) . . . 14_464 ? O3 Y1 O3 P1 -101.7(9) 11_466 . . 18_356 ? O3 Y1 O3 P1 163.9(8) 8_656 . . 18_356 ? O1 Y1 O3 P1 -12.4(8) . . . 18_356 ? O1 Y1 O3 P1 67.8(10) 11_466 . . 18_356 ? O1 Y1 O3 P1 58.3(7) 8_656 . . 18_356 ? Y2 Y1 O3 P1 31.1(8) . . . 18_356 ? O3 P1 C1 P1 -166.5(2) 24_565 . . 14_464 ? O2 P1 C1 P1 70.4(2) 14_464 . . 14_464 ? O1 P1 C1 P1 -47.02(18) . . . 14_464 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 32.43 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.141 _refine_diff_density_min -1.372 _refine_diff_density_rms 0.227 _database_code_depnum_ccdc_archive 'CCDC 927687' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1-assynthesized _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H8 Er2 O11.50 P3' _chemical_formula_weight 655.52 _chemical_absolute_configuration unk 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M I2(1)3 _symmetry_space_group_name_Hall 'I 2b 2c 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-x+1/2, y+1, -z+1' 'x+1, -y+1, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1, -x+1, -y+1/2' '-z+1, -x+1/2, y+1' '-z+1/2, x+1, -y+1' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1, -x+1' 'y+1, -z+1, -x+1/2' '-y+1, -z+1/2, x+1' _cell_length_a 13.4618(2) _cell_length_b 13.4618(2) _cell_length_c 13.4618(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2439.55(6) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6558 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 27.90 _exptl_crystal_description prismatic _exptl_crystal_colour pink _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.570 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2392 _exptl_absorpt_coefficient_mu 14.115 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6021 _exptl_absorpt_correction_T_max 0.7655 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 21211 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0225 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 28.75 _reflns_number_total 1056 _reflns_number_gt 1013 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The following two restraints were used to control the shape of the disordered atoms: ISOR 0.01 O4b C2b ISOR 0.01 O4a C2a 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^)+(0.0293P)^2^+50.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(3) _refine_ls_number_reflns 1056 _refine_ls_number_parameters 71 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0298 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0683 _refine_ls_wR_factor_gt 0.0677 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_restrained_S_all 1.139 _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 Er1 Er 0.67702(3) 0.32298(3) 0.82298(3) 0.00958(13) Uani 1 3 d S . . Er2 Er 0.52783(3) 0.47217(3) 0.97217(3) 0.01961(17) Uani 1 3 d S . . P1 P 0.44354(16) 0.60870(16) 0.77050(16) 0.0135(4) Uani 1 1 d . . . O1 O 0.5214(4) 0.3931(4) 0.8113(4) 0.0159(11) Uani 1 1 d . . . O2 O 0.4890(7) 0.5965(6) 0.8731(5) 0.038(2) Uani 1 1 d . . . O3 O 0.3778(4) 0.6993(5) 0.7627(5) 0.0220(14) Uani 1 1 d . . . O4A O 0.3415(13) 0.4884(12) 0.8720(13) 0.045(5) Uani 0.325(13) 1 d PU . 1 O4B O 0.2775(18) 0.5164(19) 0.697(2) 0.033(7) Uani 0.175(13) 1 d PU . 2 O5 O 0.4250(7) 0.5750(7) 1.0750(7) 0.067(5) Uani 1 3 d S . . C1 C 0.3650(10) 0.5000 0.7500 0.029(3) Uani 1 2 d S . . C2A C 0.3415(13) 0.4884(12) 0.8720(13) 0.045(5) Uani 0.325(13) 1 d PU . 1 C2B C 0.2775(18) 0.5164(19) 0.697(2) 0.033(7) Uani 0.175(13) 1 d PU . 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 Er1 0.00958(13) 0.00958(13) 0.00958(13) 0.00169(13) -0.00169(13) -0.00169(13) Er2 0.01961(17) 0.01961(17) 0.01961(17) -0.00085(15) 0.00085(15) 0.00085(15) P1 0.0134(10) 0.0114(9) 0.0156(10) 0.0065(8) 0.0037(8) 0.0071(8) O1 0.012(3) 0.015(3) 0.020(3) 0.001(2) -0.005(2) 0.002(2) O2 0.064(6) 0.027(4) 0.023(3) -0.006(3) -0.014(4) 0.028(4) O3 0.018(3) 0.017(3) 0.031(4) 0.012(3) 0.004(3) 0.012(2) O4A 0.058(7) 0.034(6) 0.043(7) 0.003(5) 0.017(5) 0.003(5) O4B 0.023(9) 0.033(9) 0.043(10) 0.003(6) -0.013(6) 0.003(6) O5 0.067(5) 0.067(5) 0.067(5) -0.027(4) 0.027(4) 0.027(4) C1 0.010(5) 0.022(7) 0.056(10) 0.019(6) 0.000 0.000 C2A 0.058(7) 0.034(6) 0.043(7) 0.003(5) 0.017(5) 0.003(5) C2B 0.023(9) 0.033(9) 0.043(10) 0.003(6) -0.013(6) 0.003(6) _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 Er1 O3 2.156(6) 3_646 ? Er1 O3 2.156(6) 12_665 ? Er1 O3 2.156(6) 5 ? Er1 O1 2.303(6) . ? Er1 O1 2.303(6) 7_665 ? Er1 O1 2.303(6) 10_646 ? Er1 Er2 3.4786(9) . ? Er2 O2 2.202(7) 7_665 ? Er2 O2 2.202(7) 10_646 ? Er2 O2 2.202(7) . ? Er2 O5 2.397(15) . ? Er2 O1 2.414(6) . ? Er2 O1 2.414(6) 7_665 ? Er2 O1 2.414(6) 10_646 ? Er2 C2A 2.856(19) 7_665 ? Er2 O4A 2.856(19) 7_665 ? Er2 C2A 2.856(19) 10_646 ? Er2 O4A 2.856(19) 10_646 ? Er2 O4A 2.856(19) . ? P1 O3 1.511(6) . ? P1 O1 1.521(6) 16_456 ? P1 O2 1.520(7) . ? P1 C1 1.826(8) . ? O1 P1 1.521(6) 16_456 ? O3 Er1 2.156(6) 3_656 ? O4A C1 1.680(16) . ? O4B C1 1.40(2) . ? O4B C2B 1.50(5) 16_456 ? O4B O4B 1.50(5) 16_456 ? C1 C2B 1.40(2) 16_456 ? C1 O4B 1.40(2) 16_456 ? C1 C2A 1.680(16) 16_456 ? C1 O4A 1.680(16) 16_456 ? C1 P1 1.826(8) 16_456 ? 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 Er1 O3 91.9(2) 3_646 12_665 ? O3 Er1 O3 91.9(2) 3_646 5 ? O3 Er1 O3 91.9(2) 12_665 5 ? O3 Er1 O1 88.2(2) 3_646 . ? O3 Er1 O1 160.9(2) 12_665 . ? O3 Er1 O1 107.1(2) 5 . ? O3 Er1 O1 160.9(2) 3_646 7_665 ? O3 Er1 O1 107.1(2) 12_665 7_665 ? O3 Er1 O1 88.2(2) 5 7_665 ? O1 Er1 O1 73.6(2) . 7_665 ? O3 Er1 O1 107.1(2) 3_646 10_646 ? O3 Er1 O1 88.2(2) 12_665 10_646 ? O3 Er1 O1 160.9(2) 5 10_646 ? O1 Er1 O1 73.6(2) . 10_646 ? O1 Er1 O1 73.6(2) 7_665 10_646 ? O3 Er1 Er2 123.88(17) 3_646 . ? O3 Er1 Er2 123.88(17) 12_665 . ? O3 Er1 Er2 123.88(17) 5 . ? O1 Er1 Er2 43.74(15) . . ? O1 Er1 Er2 43.74(15) 7_665 . ? O1 Er1 Er2 43.74(15) 10_646 . ? O2 Er2 O2 115.05(14) 7_665 10_646 ? O2 Er2 O2 115.05(14) 7_665 . ? O2 Er2 O2 115.05(14) 10_646 . ? O2 Er2 O5 76.94(19) 7_665 . ? O2 Er2 O5 76.94(19) 10_646 . ? O2 Er2 O5 76.94(19) . . ? O2 Er2 O1 143.9(2) 7_665 . ? O2 Er2 O1 85.3(3) 10_646 . ? O2 Er2 O1 77.5(2) . . ? O5 Er2 O1 138.73(14) . . ? O2 Er2 O1 77.5(2) 7_665 7_665 ? O2 Er2 O1 143.9(2) 10_646 7_665 ? O2 Er2 O1 85.3(3) . 7_665 ? O5 Er2 O1 138.73(14) . 7_665 ? O1 Er2 O1 69.7(2) . 7_665 ? O2 Er2 O1 85.3(3) 7_665 10_646 ? O2 Er2 O1 77.5(2) 10_646 10_646 ? O2 Er2 O1 143.9(2) . 10_646 ? O5 Er2 O1 138.73(14) . 10_646 ? O1 Er2 O1 69.7(2) . 10_646 ? O1 Er2 O1 69.7(2) 7_665 10_646 ? O2 Er2 C2A 56.5(4) 7_665 7_665 ? O2 Er2 C2A 150.7(4) 10_646 7_665 ? O2 Er2 C2A 59.4(4) . 7_665 ? O5 Er2 C2A 73.8(3) . 7_665 ? O1 Er2 C2A 118.2(4) . 7_665 ? O1 Er2 C2A 65.1(4) 7_665 7_665 ? O1 Er2 C2A 125.2(3) 10_646 7_665 ? O2 Er2 O4A 56.5(4) 7_665 7_665 ? O2 Er2 O4A 150.7(4) 10_646 7_665 ? O2 Er2 O4A 59.4(4) . 7_665 ? O5 Er2 O4A 73.8(3) . 7_665 ? O1 Er2 O4A 118.2(4) . 7_665 ? O1 Er2 O4A 65.1(4) 7_665 7_665 ? O1 Er2 O4A 125.2(3) 10_646 7_665 ? C2A Er2 O4A 0.0(7) 7_665 7_665 ? O2 Er2 C2A 59.4(4) 7_665 10_646 ? O2 Er2 C2A 56.5(4) 10_646 10_646 ? O2 Er2 C2A 150.7(4) . 10_646 ? O5 Er2 C2A 73.8(3) . 10_646 ? O1 Er2 C2A 125.2(3) . 10_646 ? O1 Er2 C2A 118.2(4) 7_665 10_646 ? O1 Er2 C2A 65.1(4) 10_646 10_646 ? C2A Er2 C2A 112.5(3) 7_665 10_646 ? O4A Er2 C2A 112.5(3) 7_665 10_646 ? O2 Er2 O4A 59.4(4) 7_665 10_646 ? O2 Er2 O4A 56.5(4) 10_646 10_646 ? O2 Er2 O4A 150.7(4) . 10_646 ? O5 Er2 O4A 73.8(3) . 10_646 ? O1 Er2 O4A 125.2(3) . 10_646 ? O1 Er2 O4A 118.2(4) 7_665 10_646 ? O1 Er2 O4A 65.1(4) 10_646 10_646 ? C2A Er2 O4A 112.5(3) 7_665 10_646 ? O4A Er2 O4A 112.5(3) 7_665 10_646 ? C2A Er2 O4A 0.0(8) 10_646 10_646 ? O2 Er2 O4A 150.7(4) 7_665 . ? O2 Er2 O4A 59.4(4) 10_646 . ? O2 Er2 O4A 56.5(4) . . ? O5 Er2 O4A 73.8(3) . . ? O1 Er2 O4A 65.1(4) . . ? O1 Er2 O4A 125.2(3) 7_665 . ? O1 Er2 O4A 118.2(4) 10_646 . ? C2A Er2 O4A 112.5(3) 7_665 . ? O4A Er2 O4A 112.5(3) 7_665 . ? C2A Er2 O4A 112.5(3) 10_646 . ? O4A Er2 O4A 112.5(3) 10_646 . ? O3 P1 O1 111.5(4) . 16_456 ? O3 P1 O2 112.7(4) . . ? O1 P1 O2 112.3(4) 16_456 . ? O3 P1 C1 107.3(4) . . ? O1 P1 C1 106.1(3) 16_456 . ? O2 P1 C1 106.5(4) . . ? P1 O1 Er1 132.0(4) 16_456 . ? P1 O1 Er2 133.0(3) 16_456 . ? Er1 O1 Er2 95.0(2) . . ? P1 O2 Er2 136.7(5) . . ? P1 O3 Er1 149.4(4) . 3_656 ? C1 O4A Er2 107.6(9) . . ? C1 O4B C2B 57.5(12) . 16_456 ? C1 O4B O4B 57.5(12) . 16_456 ? C2B O4B O4B 0(3) 16_456 16_456 ? C2B C1 O4B 0(2) 16_456 16_456 ? C2B C1 O4B 65(2) 16_456 . ? O4B C1 O4B 65(2) 16_456 . ? C2B C1 C2A 110.9(15) 16_456 16_456 ? O4B C1 C2A 110.9(15) 16_456 16_456 ? O4B C1 C2A 47.5(12) . 16_456 ? C2B C1 O4A 110.9(15) 16_456 16_456 ? O4B C1 O4A 110.9(15) 16_456 16_456 ? O4B C1 O4A 47.5(12) . 16_456 ? C2A C1 O4A 0.0(12) 16_456 16_456 ? C2B C1 O4A 47.5(12) 16_456 . ? O4B C1 O4A 47.5(12) 16_456 . ? O4B C1 O4A 110.9(15) . . ? C2A C1 O4A 158.3(15) 16_456 . ? O4A C1 O4A 158.3(15) 16_456 . ? C2B C1 P1 116.1(11) 16_456 16_456 ? O4B C1 P1 116.1(11) 16_456 16_456 ? O4B C1 P1 122.5(11) . 16_456 ? C2A C1 P1 92.1(6) 16_456 16_456 ? O4A C1 P1 92.1(6) 16_456 16_456 ? O4A C1 P1 100.5(6) . 16_456 ? C2B C1 P1 122.5(11) 16_456 . ? O4B C1 P1 122.5(11) 16_456 . ? O4B C1 P1 116.1(11) . . ? C2A C1 P1 100.5(6) 16_456 . ? O4A C1 P1 100.5(6) 16_456 . ? O4A C1 P1 92.1(6) . . ? P1 C1 P1 109.2(7) 16_456 . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 28.75 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.228 _refine_diff_density_min -2.118 _refine_diff_density_rms 0.227 _database_code_depnum_ccdc_archive 'CCDC 927688' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_publication_text _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Er2 O10.50 P3' _chemical_formula_weight 595.43 _chemical_absolute_configuration unk loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M I2(1)3 _symmetry_space_group_name_Hall 'I 2b 2c 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-x+1/2, y+1, -z+1' 'x+1, -y+1, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1, -x+1, -y+1/2' '-z+1, -x+1/2, y+1' '-z+1/2, x+1, -y+1' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1, -x+1' 'y+1, -z+1, -x+1/2' '-y+1, -z+1/2, x+1' _cell_length_a 13.4291(3) _cell_length_b 13.4291(3) _cell_length_c 13.4291(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2421.81(9) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6970 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 41.14 _exptl_crystal_description cubic _exptl_crystal_colour pink _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.266 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 14.195 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2807 _exptl_absorpt_correction_T_max 0.3310 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 21818 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 39.35 _reflns_number_total 2413 _reflns_number_gt 2303 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0301P)^2^+14.9376P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.013(15) _refine_ls_number_reflns 2413 _refine_ls_number_parameters 48 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0263 _refine_ls_R_factor_gt 0.0242 _refine_ls_wR_factor_ref 0.0605 _refine_ls_wR_factor_gt 0.0597 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 Er1 Er 0.958857(12) 0.458857(12) 0.041143(12) 0.00908(5) Uani 1 3 d S . . Er2 Er 0.809351(11) 0.309351(11) 0.190649(11) 0.00656(5) Uani 1 3 d S . . P1 P 0.72282(7) 0.54888(7) 0.10296(7) 0.00831(14) Uani 1 1 d . . . O1 O 0.7999(2) 0.4640(2) 0.1122(2) 0.0111(4) Uani 1 1 d . . . O2 O 0.6832(2) 0.2346(2) 0.1255(2) 0.0124(5) Uani 1 1 d . . . O3 O 0.8812(2) 0.5082(3) -0.0917(2) 0.0137(5) Uani 1 1 d . . . O4 O 0.7500 0.6048(3) 0.0000 0.0117(6) Uani 1 2 d S . . 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 Er1 0.00908(5) 0.00908(5) 0.00908(5) -0.00053(5) -0.00053(5) 0.00053(5) Er2 0.00656(5) 0.00656(5) 0.00656(5) -0.00026(4) -0.00026(4) 0.00026(4) P1 0.0100(3) 0.0080(3) 0.0070(3) -0.0009(3) -0.0015(3) 0.0011(3) O1 0.0106(10) 0.0109(10) 0.0116(10) 0.0003(8) 0.0011(8) 0.0051(9) O2 0.0092(11) 0.0157(12) 0.0123(11) 0.0002(9) -0.0033(9) -0.0027(9) O3 0.0089(11) 0.0197(13) 0.0124(11) 0.0038(9) 0.0000(8) 0.0001(9) O4 0.0209(18) 0.0068(14) 0.0073(14) 0.000 -0.0014(12) 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 Er1 O3 2.170(3) 11_556 ? Er1 O3 2.170(3) 8_645 ? Er1 O3 2.170(3) . ? Er1 O1 2.339(3) . ? Er1 O1 2.339(3) 8_645 ? Er1 O1 2.339(3) 11_556 ? Er1 Er2 3.4775(4) . ? Er2 O2 2.155(3) . ? Er2 O2 2.155(3) 11_556 ? Er2 O2 2.155(3) 8_645 ? Er2 O1 2.332(3) . ? Er2 O1 2.332(3) 11_556 ? Er2 O1 2.332(3) 8_645 ? P1 O2 1.498(3) 21_554 ? P1 O3 1.507(3) 15_644 ? P1 O1 1.545(3) . ? P1 O4 1.615(2) . ? O2 P1 1.498(3) 17_544 ? O3 P1 1.507(3) 15_644 ? O4 P1 1.615(2) 15_644 ? 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 Er1 O3 106.92(8) 11_556 8_645 ? O3 Er1 O3 106.92(8) 11_556 . ? O3 Er1 O3 106.92(8) 8_645 . ? O3 Er1 O1 93.33(11) 11_556 . ? O3 Er1 O1 152.73(10) 8_645 . ? O3 Er1 O1 83.55(10) . . ? O3 Er1 O1 152.73(10) 11_556 8_645 ? O3 Er1 O1 83.55(10) 8_645 8_645 ? O3 Er1 O1 93.33(11) . 8_645 ? O1 Er1 O1 70.53(11) . 8_645 ? O3 Er1 O1 83.55(10) 11_556 11_556 ? O3 Er1 O1 93.33(11) 8_645 11_556 ? O3 Er1 O1 152.73(10) . 11_556 ? O1 Er1 O1 70.53(11) . 11_556 ? O1 Er1 O1 70.53(11) 8_645 11_556 ? O3 Er1 Er2 111.92(8) 11_556 . ? O3 Er1 Er2 111.92(8) 8_645 . ? O3 Er1 Er2 111.92(8) . . ? O1 Er1 Er2 41.81(7) . . ? O1 Er1 Er2 41.81(7) 8_645 . ? O1 Er1 Er2 41.81(7) 11_556 . ? O2 Er2 O2 98.18(10) . 11_556 ? O2 Er2 O2 98.18(10) . 8_645 ? O2 Er2 O2 98.18(10) 11_556 8_645 ? O2 Er2 O1 100.87(10) . . ? O2 Er2 O1 88.18(11) 11_556 . ? O2 Er2 O1 158.84(11) 8_645 . ? O2 Er2 O1 158.84(11) . 11_556 ? O2 Er2 O1 100.87(10) 11_556 11_556 ? O2 Er2 O1 88.18(11) 8_645 11_556 ? O1 Er2 O1 70.77(11) . 11_556 ? O2 Er2 O1 88.18(11) . 8_645 ? O2 Er2 O1 158.84(11) 11_556 8_645 ? O2 Er2 O1 100.87(10) 8_645 8_645 ? O1 Er2 O1 70.77(11) . 8_645 ? O1 Er2 O1 70.77(11) 11_556 8_645 ? O2 Er2 Er1 119.23(8) . . ? O2 Er2 Er1 119.23(8) 11_556 . ? O2 Er2 Er1 119.23(8) 8_645 . ? O1 Er2 Er1 41.96(7) . . ? O1 Er2 Er1 41.96(7) 11_556 . ? O1 Er2 Er1 41.96(7) 8_645 . ? O2 P1 O3 114.80(17) 21_554 15_644 ? O2 P1 O1 112.20(16) 21_554 . ? O3 P1 O1 111.20(18) 15_644 . ? O2 P1 O4 105.79(18) 21_554 . ? O3 P1 O4 106.98(14) 15_644 . ? O1 P1 O4 105.10(15) . . ? P1 O1 Er2 136.86(17) . . ? P1 O1 Er1 126.91(17) . . ? Er2 O1 Er1 96.23(10) . . ? P1 O2 Er2 153.34(19) 17_544 . ? P1 O3 Er1 129.70(18) 15_644 . ? P1 O4 P1 124.6(3) 15_644 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 39.35 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.464 _refine_diff_density_min -3.644 _refine_diff_density_rms 0.239 _database_code_depnum_ccdc_archive 'CCDC 927689' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_publication_text _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C1.50 H1.50 Er2 O9 P3' _chemical_formula_weight 590.96 _chemical_absolute_configuration unk 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M I2(1)3 _symmetry_space_group_name_Hall 'I 2b 2c 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-x+1/2, y+1, -z+1' 'x+1, -y+1, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1, -x+1, -y+1/2' '-z+1, -x+1/2, y+1' '-z+1/2, x+1, -y+1' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1, -x+1' 'y+1, -z+1, -x+1/2' '-y+1, -z+1/2, x+1' _cell_length_a 13.43150(10) _cell_length_b 13.43150(10) _cell_length_c 13.43150(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2423.11(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9941 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 33.10 _exptl_crystal_description cubic _exptl_crystal_colour pink _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2108 _exptl_absorpt_coefficient_mu 14.177 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1846 _exptl_absorpt_correction_T_max 0.2100 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17144 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0164 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 32.57 _reflns_number_total 1488 _reflns_number_gt 1467 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; ISOR 0.005 C1: this line was used to restrain C1 atom. 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^)+(0.0451P)^2^+23.1415P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 1488 _refine_ls_number_parameters 48 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0257 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0779 _refine_ls_wR_factor_gt 0.0777 _refine_ls_goodness_of_fit_ref 1.215 _refine_ls_restrained_S_all 1.213 _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 Er1 Er 0.438149(17) 0.561851(17) 0.061851(17) 0.00852(9) Uani 1 3 d S . . Er2 Er 0.28985(2) 0.71015(2) 0.21015(2) 0.01321(11) Uani 1 3 d S . . P1 P 0.19933(11) 0.47305(11) 0.14508(11) 0.0099(2) Uani 1 1 d . . . O1 O 0.2837(4) 0.5517(3) 0.1381(3) 0.0147(8) Uani 1 1 d . . . O2 O 0.1570(3) 0.7585(4) 0.1307(3) 0.0152(8) Uani 1 1 d . . . O3 O 0.3743(3) 0.4820(3) -0.0623(4) 0.0178(8) Uani 1 1 d . . . C1 C 0.1396(6) 0.5000 0.2500 0.0098(12) Uani 1 2 d SU . . H1 H 0.0689 0.5000 0.2500 0.012 Uiso 1 2 calc SR . . 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 Er1 0.00852(9) 0.00852(9) 0.00852(9) 0.00148(8) -0.00148(8) -0.00148(8) Er2 0.01321(11) 0.01321(11) 0.01321(11) 0.00236(9) -0.00236(9) -0.00236(9) P1 0.0098(6) 0.0106(5) 0.0092(5) 0.0026(4) -0.0010(5) -0.0014(5) O1 0.0183(19) 0.0115(17) 0.0144(17) -0.0010(14) 0.0012(15) -0.0076(16) O2 0.0104(17) 0.023(2) 0.0123(18) 0.0014(16) -0.0013(14) 0.0069(16) O3 0.0152(18) 0.017(2) 0.021(2) -0.0059(18) -0.0093(18) 0.0038(15) C1 0.013(3) 0.013(3) 0.003(2) -0.001(2) 0.000 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 Er1 O3 2.161(5) . ? Er1 O3 2.161(5) 7_564 ? Er1 O3 2.161(5) 10_655 ? Er1 O1 2.318(5) . ? Er1 O1 2.318(5) 10_655 ? Er1 O1 2.318(5) 7_564 ? Er1 Er2 3.4499(6) . ? Er2 O2 2.178(4) . ? Er2 O2 2.178(4) 7_564 ? Er2 O2 2.178(4) 10_655 ? Er2 O1 2.340(4) 10_655 ? Er2 O1 2.340(4) 7_564 ? Er2 O1 2.340(4) . ? P1 O3 1.492(5) 15_544 ? P1 O2 1.513(5) 24_554 ? P1 O1 1.552(4) . ? P1 C1 1.661(4) . ? O2 P1 1.513(5) 18_455 ? O3 P1 1.492(5) 15_544 ? C1 P1 1.661(4) 16_455 ? C1 H1 0.9500 . ? 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 Er1 O3 96.92(16) . 7_564 ? O3 Er1 O3 96.92(16) . 10_655 ? O3 Er1 O3 96.92(16) 7_564 10_655 ? O3 Er1 O1 87.50(18) . . ? O3 Er1 O1 159.03(18) 7_564 . ? O3 Er1 O1 102.91(16) 10_655 . ? O3 Er1 O1 159.03(18) . 10_655 ? O3 Er1 O1 102.91(16) 7_564 10_655 ? O3 Er1 O1 87.50(17) 10_655 10_655 ? O1 Er1 O1 71.53(17) . 10_655 ? O3 Er1 O1 102.91(16) . 7_564 ? O3 Er1 O1 87.50(18) 7_564 7_564 ? O3 Er1 O1 159.03(18) 10_655 7_564 ? O1 Er1 O1 71.54(17) . 7_564 ? O1 Er1 O1 71.53(17) 10_655 7_564 ? O3 Er1 Er2 120.20(12) . . ? O3 Er1 Er2 120.20(12) 7_564 . ? O3 Er1 Er2 120.20(12) 10_655 . ? O1 Er1 Er2 42.45(11) . . ? O1 Er1 Er2 42.45(11) 10_655 . ? O1 Er1 Er2 42.45(11) 7_564 . ? O2 Er2 O2 107.64(12) . 7_564 ? O2 Er2 O2 107.64(12) . 10_655 ? O2 Er2 O2 107.64(12) 7_564 10_655 ? O2 Er2 O1 152.38(16) . 10_655 ? O2 Er2 O1 83.27(16) 7_564 10_655 ? O2 Er2 O1 92.27(17) 10_655 10_655 ? O2 Er2 O1 83.27(16) . 7_564 ? O2 Er2 O1 92.27(17) 7_564 7_564 ? O2 Er2 O1 152.38(16) 10_655 7_564 ? O1 Er2 O1 70.77(18) 10_655 7_564 ? O2 Er2 O1 92.27(17) . . ? O2 Er2 O1 152.38(16) 7_564 . ? O2 Er2 O1 83.27(16) 10_655 . ? O1 Er2 O1 70.77(18) 10_655 . ? O1 Er2 O1 70.77(18) 7_564 . ? O2 Er2 Er1 111.25(12) . . ? O2 Er2 Er1 111.25(12) 7_564 . ? O2 Er2 Er1 111.25(12) 10_655 . ? O1 Er2 Er1 41.96(11) 10_655 . ? O1 Er2 Er1 41.96(11) 7_564 . ? O1 Er2 Er1 41.96(11) . . ? O3 P1 O2 113.6(3) 15_544 24_554 ? O3 P1 O1 112.6(3) 15_544 . ? O2 P1 O1 111.1(3) 24_554 . ? O3 P1 C1 107.1(3) 15_544 . ? O2 P1 C1 107.0(2) 24_554 . ? O1 P1 C1 104.8(3) . . ? P1 O1 Er1 136.1(3) . . ? P1 O1 Er2 128.3(3) . . ? Er1 O1 Er2 95.59(15) . . ? P1 O2 Er2 130.5(3) 18_455 . ? P1 O3 Er1 151.4(3) 15_544 . ? P1 C1 P1 122.3(5) 16_455 . ? P1 C1 H1 118.9 16_455 . ? P1 C1 H1 118.9 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 32.57 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.388 _refine_diff_density_min -4.052 _refine_diff_density_rms 0.275 _database_code_depnum_ccdc_archive 'CCDC 927690' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_publication_text _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C H3 Er2 O11.50 P3' _chemical_formula_weight 626.46 _chemical_absolute_configuration unk 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M I2(1)3 _symmetry_space_group_name_Hall 'I 2b 2c 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-x+1/2, y+1, -z+1' 'x+1, -y+1, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1, -x+1, -y+1/2' '-z+1, -x+1/2, y+1' '-z+1/2, x+1, -y+1' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1, -x+1' 'y+1, -z+1, -x+1/2' '-y+1, -z+1/2, x+1' _cell_length_a 13.4154(2) _cell_length_b 13.4154(2) _cell_length_c 13.4154(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2414.41(6) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4634 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 27.99 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2256 _exptl_absorpt_coefficient_mu 14.253 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3298 _exptl_absorpt_correction_T_max 0.3951 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14034 _diffrn_reflns_av_R_equivalents 0.0762 _diffrn_reflns_av_sigmaI/netI 0.0640 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 30.45 _reflns_number_total 1232 _reflns_number_gt 912 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; During the refinement, some restraints were used to fix methanol atom: DFIX 1.418 0.001 O1M C1M ISOR 0.01 C1M EQIV $1 1-z, 0.5+x, 1.5-y EQIV $2 -0.5+y, 1.5-z, 1-x FREE C1M C1M_$1 FREE C1M C1M_$2. 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^)+(0.0357P)^2^+72.6784P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(5) _refine_ls_number_reflns 1232 _refine_ls_number_parameters 61 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0828 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.1034 _refine_ls_wR_factor_gt 0.0838 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_restrained_S_all 1.140 _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 Er1 Er 0.18513(4) 0.68513(4) 0.81487(4) 0.0175(2) Uani 1 3 d S . . Er2 Er 0.03164(4) 0.53164(4) 0.96836(4) 0.0232(3) Uani 1 3 d S . . P1 P 0.2714(3) 0.4480(3) 0.8955(3) 0.0200(6) Uani 1 1 d . . . O1 O 0.1919(7) 0.5284(7) 0.8866(6) 0.0229(18) Uani 1 1 d . . . O2 O 0.3743(7) 0.4935(8) 0.9030(7) 0.030(2) Uani 1 1 d . . . O3 O 0.2500 0.3932(10) 1.0000 0.031(3) Uani 1 2 d S . . O4 O 0.2626(7) 0.3700(7) 0.8183(8) 0.025(2) Uani 1 1 d . . . O1M O -0.0698(8) 0.4302(8) 1.0698(8) 0.064(7) Uani 1 3 d SD . . C1M C -0.045(4) 0.3323(17) 1.101(4) 0.043(13) Uani 0.33 1 d PDU . . H1M1 H -0.1051 0.2904 1.0988 0.065 Uiso 0.33 1 calc PR . . H1M2 H -0.0197 0.3344 1.1695 0.065 Uiso 0.33 1 calc PR . . H1M3 H 0.0056 0.3045 1.0569 0.065 Uiso 0.33 1 calc PR . . 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 Er1 0.0175(2) 0.0175(2) 0.0175(2) -0.0005(2) -0.0005(2) 0.0005(2) Er2 0.0232(3) 0.0232(3) 0.0232(3) -0.0008(2) -0.0008(2) 0.0008(2) P1 0.0197(17) 0.0211(18) 0.0192(16) -0.0014(14) -0.0027(13) 0.0016(13) O1 0.024(4) 0.021(4) 0.024(4) -0.002(4) 0.003(4) 0.008(4) O2 0.032(5) 0.036(6) 0.021(5) -0.011(4) -0.003(4) -0.002(4) O3 0.055(9) 0.021(7) 0.017(7) 0.000 -0.007(6) 0.000 O4 0.021(4) 0.038(5) 0.017(4) -0.001(4) -0.004(4) 0.004(4) O1M 0.064(7) 0.064(7) 0.064(7) 0.022(6) 0.022(6) -0.022(6) C1M 0.039(15) 0.046(15) 0.045(15) 0.000(9) -0.004(9) 0.000(9) _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 Er1 O4 2.195(10) 17_455 ? Er1 O4 2.195(10) 16_456 ? Er1 O4 2.195(10) 22_545 ? Er1 O1 2.314(9) . ? Er1 O1 2.314(9) 11_466 ? Er1 O1 2.314(9) 8_656 ? Er1 Er2 3.5666(14) . ? Er2 O2 2.197(10) 21_445 ? Er2 O2 2.197(10) 15_546 ? Er2 O2 2.197(10) 18_356 ? Er2 O1M 2.356(19) . ? Er2 O1 2.414(9) . ? Er2 O1 2.414(9) 8_656 ? Er2 O1 2.414(9) 11_466 ? P1 O4 1.477(10) . ? P1 O2 1.513(10) . ? P1 O1 1.522(9) . ? P1 O3 1.609(7) . ? O2 Er2 2.198(10) 15_546 ? O3 P1 1.609(7) 15_546 ? O4 Er1 2.195(10) 16_456 ? O1M C1M 1.4180(11) 11_466 ? O1M C1M 1.4180(10) 8_656 ? O1M C1M 1.4180(10) . ? C1M H1M1 0.9800 . ? C1M H1M2 0.9800 . ? C1M H1M3 0.9800 . ? 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 Er1 O4 92.8(3) 17_455 16_456 ? O4 Er1 O4 92.8(3) 17_455 22_545 ? O4 Er1 O4 92.8(3) 16_456 22_545 ? O4 Er1 O1 105.0(3) 17_455 . ? O4 Er1 O1 90.8(3) 16_456 . ? O4 Er1 O1 161.7(3) 22_545 . ? O4 Er1 O1 161.7(3) 17_455 11_466 ? O4 Er1 O1 105.0(3) 16_456 11_466 ? O4 Er1 O1 90.8(3) 22_545 11_466 ? O1 Er1 O1 71.0(3) . 11_466 ? O4 Er1 O1 90.8(3) 17_455 8_656 ? O4 Er1 O1 161.7(3) 16_456 8_656 ? O4 Er1 O1 105.0(3) 22_545 8_656 ? O1 Er1 O1 71.0(3) . 8_656 ? O1 Er1 O1 71.0(3) 11_466 8_656 ? O4 Er1 Er2 123.3(2) 17_455 . ? O4 Er1 Er2 123.3(2) 16_456 . ? O4 Er1 Er2 123.3(2) 22_545 . ? O1 Er1 Er2 42.1(2) . . ? O1 Er1 Er2 42.1(2) 11_466 . ? O1 Er1 Er2 42.1(2) 8_656 . ? O2 Er2 O2 113.7(2) 21_445 15_546 ? O2 Er2 O2 113.7(2) 21_445 18_356 ? O2 Er2 O2 113.7(2) 15_546 18_356 ? O2 Er2 O1M 75.2(2) 21_445 . ? O2 Er2 O1M 75.2(2) 15_546 . ? O2 Er2 O1M 75.2(2) 18_356 . ? O2 Er2 O1 86.1(3) 21_445 . ? O2 Er2 O1 80.9(3) 15_546 . ? O2 Er2 O1 144.6(3) 18_356 . ? O1M Er2 O1 140.0(2) . . ? O2 Er2 O1 144.6(3) 21_445 8_656 ? O2 Er2 O1 86.1(3) 15_546 8_656 ? O2 Er2 O1 80.9(3) 18_356 8_656 ? O1M Er2 O1 140.0(2) . 8_656 ? O1 Er2 O1 67.6(3) . 8_656 ? O2 Er2 O1 80.9(3) 21_445 11_466 ? O2 Er2 O1 144.6(3) 15_546 11_466 ? O2 Er2 O1 86.1(3) 18_356 11_466 ? O1M Er2 O1 140.0(2) . 11_466 ? O1 Er2 O1 67.6(3) . 11_466 ? O1 Er2 O1 67.6(3) 8_656 11_466 ? O2 Er2 Er1 104.8(2) 21_445 . ? O2 Er2 Er1 104.8(2) 15_546 . ? O2 Er2 Er1 104.8(2) 18_356 . ? O1M Er2 Er1 180.0(2) . . ? O1 Er2 Er1 40.0(2) . . ? O1 Er2 Er1 40.0(2) 8_656 . ? O1 Er2 Er1 40.0(2) 11_466 . ? O4 P1 O2 114.0(5) . . ? O4 P1 O1 113.0(5) . . ? O2 P1 O1 111.0(6) . . ? O4 P1 O3 105.9(6) . . ? O2 P1 O3 106.8(5) . . ? O1 P1 O3 105.5(5) . . ? P1 O1 Er1 134.8(5) . . ? P1 O1 Er2 127.0(5) . . ? Er1 O1 Er2 97.9(3) . . ? P1 O2 Er2 132.1(6) . 15_546 ? P1 O3 P1 125.7(9) 15_546 . ? P1 O4 Er1 147.9(6) . 16_456 ? C1M O1M C1M 90(3) 11_466 8_656 ? C1M O1M C1M 90(3) 11_466 . ? C1M O1M C1M 90(3) 8_656 . ? C1M O1M Er2 125(2) 11_466 . ? C1M O1M Er2 125(2) 8_656 . ? C1M O1M Er2 125(2) . . ? O1M C1M H1M1 109.5 . . ? O1M C1M H1M2 109.5 . . ? H1M1 C1M H1M2 109.5 . . ? O1M C1M H1M3 109.5 . . ? H1M1 C1M H1M3 109.5 . . ? H1M2 C1M H1M3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.45 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.920 _refine_diff_density_min -2.259 _refine_diff_density_rms 0.373 _database_code_depnum_ccdc_archive 'CCDC 927691' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_publication_text _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H8 Dy2 O11.50 P3' _chemical_formula_weight 646.00 _chemical_absolute_configuration unk 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M I2(1)3 _symmetry_space_group_name_Hall 'I 2b 2c 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-x+1/2, y+1, -z+1' 'x+1, -y+1, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1, -x+1, -y+1/2' '-z+1, -x+1/2, y+1' '-z+1/2, x+1, -y+1' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1, -x+1' 'y+1, -z+1, -x+1/2' '-y+1, -z+1/2, x+1' _cell_length_a 13.5416(2) _cell_length_b 13.5416(2) _cell_length_c 13.5416(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2483.19(6) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9839 _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 39.84 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2360 _exptl_absorpt_coefficient_mu 12.385 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1908 _exptl_absorpt_correction_T_max 0.2760 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 34956 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0285 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 40.08 _reflns_number_total 2605 _reflns_number_gt 2453 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0338P)^2^+2.2838P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.019(15) _refine_ls_number_reflns 2605 _refine_ls_number_parameters 71 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0298 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0649 _refine_ls_wR_factor_gt 0.0640 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _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 Dy1 Dy 0.678583(10) 0.321417(10) 0.821417(10) 0.01153(5) Uani 1 3 d S . . Dy2 Dy 0.528509(12) 0.471491(12) 0.971491(12) 0.01771(6) Uani 1 3 d S . . P1 P 0.44526(7) 0.39160(7) 0.72902(7) 0.01700(15) Uani 1 1 d . . . O1 O 0.5224(2) 0.39175(18) 0.8110(2) 0.0187(4) Uani 1 1 d . . . O2 O 0.4919(4) 0.5975(3) 0.8724(2) 0.0480(13) Uani 1 1 d . . . O3 O 0.8025(2) 0.2363(3) 0.8788(2) 0.0268(6) Uani 1 1 d . . . O4A O 0.3529(8) 0.4881(8) 0.8763(7) 0.024(2) Uani 0.172(7) 1 d P . 1 C2A C 0.3529(8) 0.4881(8) 0.8763(7) 0.024(2) Uani 0.172(7) 1 d P . 1 O4B O 0.2625(11) 0.4896(15) 0.7879(13) 0.117(7) Uani 0.328(7) 1 d P . 2 C2B C 0.2625(11) 0.4896(15) 0.7879(13) 0.117(7) Uani 0.328(7) 1 d P . 2 O5 O 0.4255(3) 0.5745(3) 1.0745(3) 0.053(2) Uani 1 3 d S . . C1 C 0.3707(5) 0.5000 0.7500 0.048(3) Uani 1 2 d S . . 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 Dy1 0.01153(5) 0.01153(5) 0.01153(5) 0.00112(4) -0.00112(4) -0.00112(4) Dy2 0.01771(6) 0.01771(6) 0.01771(6) -0.00082(5) 0.00082(5) 0.00082(5) P1 0.0164(4) 0.0173(4) 0.0173(4) 0.0064(3) -0.0057(3) -0.0069(3) O1 0.0191(10) 0.0142(9) 0.0228(11) -0.0003(8) -0.0100(9) 0.0020(8) O2 0.097(4) 0.0276(16) 0.0198(14) 0.0003(12) -0.0104(18) 0.035(2) O3 0.0243(13) 0.0330(15) 0.0230(13) -0.0118(11) -0.0122(11) 0.0138(11) O4A 0.029(5) 0.022(4) 0.021(4) 0.004(3) 0.008(3) -0.003(4) C2A 0.029(5) 0.022(4) 0.021(4) 0.004(3) 0.008(3) -0.003(4) O4B 0.085(9) 0.165(16) 0.100(11) 0.081(12) 0.000(7) -0.035(10) C2B 0.085(9) 0.165(16) 0.100(11) 0.081(12) 0.000(7) -0.035(10) O5 0.053(2) 0.053(2) 0.053(2) -0.0158(17) 0.0158(17) 0.0158(17) C1 0.012(2) 0.027(3) 0.106(8) 0.026(4) 0.000 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 Dy1 O3 2.178(3) . ? Dy1 O3 2.178(3) 7_665 ? Dy1 O3 2.178(3) 10_646 ? Dy1 O1 2.324(3) . ? Dy1 O1 2.324(3) 7_665 ? Dy1 O1 2.324(3) 10_646 ? Dy1 Dy2 3.5199(4) . ? Dy2 O2 2.227(3) . ? Dy2 O2 2.227(3) 7_665 ? Dy2 O2 2.227(3) 10_646 ? Dy2 O5 2.416(8) . ? Dy2 O1 2.428(3) . ? Dy2 O1 2.428(3) 10_646 ? Dy2 O1 2.428(3) 7_665 ? Dy2 C2A 2.714(12) 7_665 ? Dy2 O4A 2.714(12) 7_665 ? Dy2 C2A 2.714(12) 10_646 ? Dy2 O4A 2.714(12) 10_646 ? Dy2 O4A 2.714(12) . ? P1 O3 1.509(3) 17_445 ? P1 O2 1.519(4) 16_456 ? P1 O1 1.524(3) . ? P1 C1 1.804(4) . ? O2 P1 1.519(4) 16_456 ? O3 P1 1.509(3) 21_545 ? O4A C1 1.734(10) . ? O4B C2B 1.07(3) 16_456 ? O4B O4B 1.07(3) 16_456 ? O4B C1 1.559(15) . ? C1 C2B 1.559(15) 16_456 ? C1 O4B 1.559(15) 16_456 ? C1 C2A 1.734(10) 16_456 ? C1 O4A 1.734(10) 16_456 ? C1 P1 1.804(4) 16_456 ? 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 Dy1 O3 93.20(10) . 7_665 ? O3 Dy1 O3 93.20(10) . 10_646 ? O3 Dy1 O3 93.20(10) 7_665 10_646 ? O3 Dy1 O1 159.94(12) . . ? O3 Dy1 O1 87.66(10) 7_665 . ? O3 Dy1 O1 106.77(11) 10_646 . ? O3 Dy1 O1 106.77(11) . 7_665 ? O3 Dy1 O1 159.94(12) 7_665 7_665 ? O3 Dy1 O1 87.66(10) 10_646 7_665 ? O1 Dy1 O1 72.96(10) . 7_665 ? O3 Dy1 O1 87.66(10) . 10_646 ? O3 Dy1 O1 106.77(11) 7_665 10_646 ? O3 Dy1 O1 159.94(12) 10_646 10_646 ? O1 Dy1 O1 72.96(10) . 10_646 ? O1 Dy1 O1 72.96(10) 7_665 10_646 ? O3 Dy1 Dy2 122.97(7) . . ? O3 Dy1 Dy2 122.97(7) 7_665 . ? O3 Dy1 Dy2 122.97(7) 10_646 . ? O1 Dy1 Dy2 43.36(7) . . ? O1 Dy1 Dy2 43.36(7) 7_665 . ? O1 Dy1 Dy2 43.36(6) 10_646 . ? O2 Dy2 O2 115.18(7) . 7_665 ? O2 Dy2 O2 115.18(7) . 10_646 ? O2 Dy2 O2 115.18(7) 7_665 10_646 ? O2 Dy2 O5 77.13(10) . . ? O2 Dy2 O5 77.12(10) 7_665 . ? O2 Dy2 O5 77.12(10) 10_646 . ? O2 Dy2 O1 78.09(11) . . ? O2 Dy2 O1 143.64(12) 7_665 . ? O2 Dy2 O1 84.54(16) 10_646 . ? O5 Dy2 O1 138.92(6) . . ? O2 Dy2 O1 143.64(12) . 10_646 ? O2 Dy2 O1 84.54(16) 7_665 10_646 ? O2 Dy2 O1 78.10(11) 10_646 10_646 ? O5 Dy2 O1 138.92(6) . 10_646 ? O1 Dy2 O1 69.37(10) . 10_646 ? O2 Dy2 O1 84.54(16) . 7_665 ? O2 Dy2 O1 78.10(11) 7_665 7_665 ? O2 Dy2 O1 143.64(12) 10_646 7_665 ? O5 Dy2 O1 138.92(6) . 7_665 ? O1 Dy2 O1 69.37(10) . 7_665 ? O1 Dy2 O1 69.37(10) 10_646 7_665 ? O2 Dy2 C2A 59.0(2) . 7_665 ? O2 Dy2 C2A 57.0(3) 7_665 7_665 ? O2 Dy2 C2A 150.9(2) 10_646 7_665 ? O5 Dy2 C2A 73.8(2) . 7_665 ? O1 Dy2 C2A 118.7(2) . 7_665 ? O1 Dy2 C2A 124.8(2) 10_646 7_665 ? O1 Dy2 C2A 65.3(2) 7_665 7_665 ? O2 Dy2 O4A 59.0(2) . 7_665 ? O2 Dy2 O4A 57.0(3) 7_665 7_665 ? O2 Dy2 O4A 150.9(2) 10_646 7_665 ? O5 Dy2 O4A 73.8(2) . 7_665 ? O1 Dy2 O4A 118.7(2) . 7_665 ? O1 Dy2 O4A 124.8(2) 10_646 7_665 ? O1 Dy2 O4A 65.3(2) 7_665 7_665 ? C2A Dy2 O4A 0.0(5) 7_665 7_665 ? O2 Dy2 C2A 150.9(2) . 10_646 ? O2 Dy2 C2A 59.0(2) 7_665 10_646 ? O2 Dy2 C2A 57.0(3) 10_646 10_646 ? O5 Dy2 C2A 73.8(2) . 10_646 ? O1 Dy2 C2A 124.8(2) . 10_646 ? O1 Dy2 C2A 65.3(2) 10_646 10_646 ? O1 Dy2 C2A 118.7(2) 7_665 10_646 ? C2A Dy2 C2A 112.51(18) 7_665 10_646 ? O4A Dy2 C2A 112.51(18) 7_665 10_646 ? O2 Dy2 O4A 150.9(2) . 10_646 ? O2 Dy2 O4A 59.0(2) 7_665 10_646 ? O2 Dy2 O4A 57.0(3) 10_646 10_646 ? O5 Dy2 O4A 73.8(2) . 10_646 ? O1 Dy2 O4A 124.8(2) . 10_646 ? O1 Dy2 O4A 65.3(2) 10_646 10_646 ? O1 Dy2 O4A 118.7(2) 7_665 10_646 ? C2A Dy2 O4A 112.51(18) 7_665 10_646 ? O4A Dy2 O4A 112.51(18) 7_665 10_646 ? C2A Dy2 O4A 0.0(6) 10_646 10_646 ? O2 Dy2 O4A 57.0(3) . . ? O2 Dy2 O4A 150.9(2) 7_665 . ? O2 Dy2 O4A 59.0(2) 10_646 . ? O5 Dy2 O4A 73.8(2) . . ? O1 Dy2 O4A 65.3(2) . . ? O1 Dy2 O4A 118.7(2) 10_646 . ? O1 Dy2 O4A 124.8(2) 7_665 . ? C2A Dy2 O4A 112.51(18) 7_665 . ? O4A Dy2 O4A 112.51(18) 7_665 . ? C2A Dy2 O4A 112.51(18) 10_646 . ? O4A Dy2 O4A 112.51(18) 10_646 . ? O3 P1 O2 112.7(2) 17_445 16_456 ? O3 P1 O1 111.22(15) 17_445 . ? O2 P1 O1 111.9(2) 16_456 . ? O3 P1 C1 107.8(2) 17_445 . ? O2 P1 C1 107.2(2) 16_456 . ? O1 P1 C1 105.53(16) . . ? P1 O1 Dy1 131.85(16) . . ? P1 O1 Dy2 132.53(16) . . ? Dy1 O1 Dy2 95.56(9) . . ? P1 O2 Dy2 135.4(3) 16_456 . ? P1 O3 Dy1 149.7(2) 21_545 . ? C1 O4A Dy2 110.8(5) . . ? C2B O4B O4B 0.0(16) 16_456 16_456 ? C2B O4B C1 70.0(6) 16_456 . ? O4B O4B C1 70.0(6) 16_456 . ? C2B C1 O4B 0.0(4) 16_456 16_456 ? C2B C1 O4B 40.0(11) 16_456 . ? O4B C1 O4B 40.0(11) 16_456 . ? C2B C1 O4A 101.7(8) 16_456 . ? O4B C1 O4A 101.7(8) 16_456 . ? O4B C1 O4A 62.4(7) . . ? C2B C1 C2A 62.4(7) 16_456 16_456 ? O4B C1 C2A 62.4(7) 16_456 16_456 ? O4B C1 C2A 101.7(8) . 16_456 ? O4A C1 C2A 164.1(9) . 16_456 ? C2B C1 O4A 62.4(7) 16_456 16_456 ? O4B C1 O4A 62.4(7) 16_456 16_456 ? O4B C1 O4A 101.7(8) . 16_456 ? O4A C1 O4A 164.1(9) . 16_456 ? C2A C1 O4A 0.0(7) 16_456 16_456 ? C2B C1 P1 123.2(9) 16_456 . ? O4B C1 P1 123.2(9) 16_456 . ? O4B C1 P1 120.3(8) . . ? O4A C1 P1 99.1(4) . . ? C2A C1 P1 89.9(4) 16_456 . ? O4A C1 P1 89.9(4) 16_456 . ? C2B C1 P1 120.3(8) 16_456 16_456 ? O4B C1 P1 120.3(8) 16_456 16_456 ? O4B C1 P1 123.2(9) . 16_456 ? O4A C1 P1 89.9(4) . 16_456 ? C2A C1 P1 99.1(4) 16_456 16_456 ? O4A C1 P1 99.1(4) 16_456 16_456 ? P1 C1 P1 111.9(3) . 16_456 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 40.08 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.871 _refine_diff_density_min -2.219 _refine_diff_density_rms 0.230 _database_code_depnum_ccdc_archive 'CCDC 934836' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_publication_text _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H8 O11.50 P3 Tb2' _chemical_formula_weight 638.84 _chemical_absolute_configuration unk 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' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M I2(1)3 _symmetry_space_group_name_Hall 'I 2b 2c 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-x+1/2, y+1, -z+1' 'x+1, -y+1, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1, -x+1, -y+1/2' '-z+1, -x+1/2, y+1' '-z+1/2, x+1, -y+1' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1, -x+1' 'y+1, -z+1, -x+1/2' '-y+1, -z+1/2, x+1' _cell_length_a 13.61780(10) _cell_length_b 13.61780(10) _cell_length_c 13.61780(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2525.35(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5191 _cell_measurement_theta_min 3.66 _cell_measurement_theta_max 34.29 _exptl_crystal_description cubic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 11.545 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4586 _exptl_absorpt_correction_T_max 0.5442 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14555 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.66 _diffrn_reflns_theta_max 36.27 _reflns_number_total 2041 _reflns_number_gt 1852 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0262P)^2^+4.9161P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.010(18) _refine_ls_number_reflns 2041 _refine_ls_number_parameters 70 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0244 _refine_ls_wR_factor_ref 0.0555 _refine_ls_wR_factor_gt 0.0531 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.128 _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 Tb1 Tb 0.821198(12) 0.321198(12) 0.178802(12) 0.01271(6) Uani 1 3 d S . . Tb2 Tb 0.971550(14) 0.471550(14) 0.028450(14) 0.01804(7) Uani 1 3 d S . . P1 P 0.89167(8) 0.22927(8) -0.05478(8) 0.01815(18) Uani 1 1 d . . . O1 O 0.8913(2) 0.3107(2) 0.0221(2) 0.0193(5) Uani 1 1 d . . . O2 O 1.0079(5) 0.5978(3) 0.1289(3) 0.0492(14) Uani 1 1 d . . . O3 O 0.8790(2) 0.1970(3) 0.2639(3) 0.0299(8) Uani 1 1 d . . . O4A O 0.9815(11) 0.2858(12) -0.2270(8) 0.061(5) Uani 0.223(8) 1 d P . 1 C2A C 0.9815(11) 0.2858(12) -0.2270(8) 0.061(5) Uani 0.223(8) 1 d P . 1 O4B O 1.0104(8) 0.1240(7) -0.1494(8) 0.044(3) Uani 0.277(8) 1 d P . 2 C2B C 1.0104(8) 0.1240(7) -0.1494(8) 0.044(3) Uani 0.277(8) 1 d P . 2 O5 O 1.0750(3) 0.5750(3) -0.0750(3) 0.061(3) Uani 1 3 d S . . C1 C 1.0000 0.2500 -0.1301(5) 0.050(3) Uani 1 2 d S . . 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 0.01271(6) 0.01271(6) 0.01271(6) -0.00175(6) -0.00175(6) 0.00175(6) Tb2 0.01804(7) 0.01804(7) 0.01804(7) 0.00011(6) 0.00011(6) -0.00011(6) P1 0.0201(5) 0.0181(4) 0.0163(4) -0.0060(3) -0.0081(3) 0.0081(4) O1 0.0176(11) 0.0232(13) 0.0171(12) -0.0101(11) 0.0010(9) 0.0007(10) O2 0.096(4) 0.0291(19) 0.0228(16) -0.0009(14) -0.011(2) -0.037(2) O3 0.0222(15) 0.0286(17) 0.0389(19) 0.0158(15) 0.0123(13) 0.0111(13) O4A 0.067(9) 0.092(12) 0.026(5) 0.029(6) 0.010(5) 0.043(8) C2A 0.067(9) 0.092(12) 0.026(5) 0.029(6) 0.010(5) 0.043(8) O4B 0.045(5) 0.038(5) 0.051(6) -0.009(4) 0.006(4) 0.003(4) C2B 0.045(5) 0.038(5) 0.051(6) -0.009(4) 0.006(4) 0.003(4) O5 0.061(3) 0.061(3) 0.061(3) 0.020(2) 0.020(2) -0.020(2) C1 0.031(4) 0.108(9) 0.012(3) 0.000 0.000 0.033(5) _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 2.196(3) . ? Tb1 O3 2.196(3) 11_556 ? Tb1 O3 2.196(3) 8_645 ? Tb1 O1 2.343(3) 8_645 ? Tb1 O1 2.343(3) 11_556 ? Tb1 O1 2.343(3) . ? Tb1 Tb2 3.5463(4) . ? Tb2 O2 2.252(4) 8_645 ? Tb2 O2 2.251(4) 11_556 ? Tb2 O2 2.252(4) . ? Tb2 O5 2.439(8) . ? Tb2 O1 2.449(3) . ? Tb2 O1 2.449(3) 8_645 ? Tb2 O1 2.449(3) 11_556 ? Tb2 C2B 2.760(11) 19_564 ? Tb2 O4B 2.760(11) 19_564 ? Tb2 C2B 2.760(11) 14_654 ? Tb2 O4B 2.760(11) 14_654 ? Tb2 C2B 2.760(11) 24_553 ? P1 O3 1.510(3) 24_553 ? P1 O2 1.516(4) 22_645 ? P1 O1 1.525(3) . ? P1 C1 1.818(4) . ? O2 P1 1.516(4) 19_564 ? O3 P1 1.510(3) 18 ? O4A C2A 1.10(3) 14_654 ? O4A O4A 1.10(3) 14_654 ? O4A C1 1.429(11) . ? O4B C1 1.742(10) . ? O4B Tb2 2.760(11) 14_654 ? C1 C2A 1.429(11) 14_654 ? C1 O4A 1.429(11) 14_654 ? C1 C2B 1.742(10) 14_654 ? C1 O4B 1.742(10) 14_654 ? C1 P1 1.818(4) 14_654 ? 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 O3 93.39(11) . 11_556 ? O3 Tb1 O3 93.39(11) . 8_645 ? O3 Tb1 O3 93.39(11) 11_556 8_645 ? O3 Tb1 O1 87.43(11) . 8_645 ? O3 Tb1 O1 159.81(13) 11_556 8_645 ? O3 Tb1 O1 106.72(12) 8_645 8_645 ? O3 Tb1 O1 159.81(13) . 11_556 ? O3 Tb1 O1 106.72(12) 11_556 11_556 ? O3 Tb1 O1 87.43(11) 8_645 11_556 ? O1 Tb1 O1 73.07(11) 8_645 11_556 ? O3 Tb1 O1 106.72(12) . . ? O3 Tb1 O1 87.43(11) 11_556 . ? O3 Tb1 O1 159.80(13) 8_645 . ? O1 Tb1 O1 73.07(11) 8_645 . ? O1 Tb1 O1 73.07(11) 11_556 . ? O3 Tb1 Tb2 122.83(8) . . ? O3 Tb1 Tb2 122.83(8) 11_556 . ? O3 Tb1 Tb2 122.83(8) 8_645 . ? O1 Tb1 Tb2 43.42(7) 8_645 . ? O1 Tb1 Tb2 43.42(7) 11_556 . ? O1 Tb1 Tb2 43.42(7) . . ? O2 Tb2 O2 115.43(8) 8_645 11_556 ? O2 Tb2 O2 115.43(8) 8_645 . ? O2 Tb2 O2 115.43(8) 11_556 . ? O2 Tb2 O5 77.47(11) 8_645 . ? O2 Tb2 O5 77.47(11) 11_556 . ? O2 Tb2 O5 77.46(11) . . ? O2 Tb2 O1 84.19(16) 8_645 . ? O2 Tb2 O1 77.84(12) 11_556 . ? O2 Tb2 O1 143.35(13) . . ? O5 Tb2 O1 138.88(7) . . ? O2 Tb2 O1 143.35(13) 8_645 8_645 ? O2 Tb2 O1 84.19(16) 11_556 8_645 ? O2 Tb2 O1 77.84(12) . 8_645 ? O5 Tb2 O1 138.88(7) . 8_645 ? O1 Tb2 O1 69.43(11) . 8_645 ? O2 Tb2 O1 77.84(12) 8_645 11_556 ? O2 Tb2 O1 143.35(13) 11_556 11_556 ? O2 Tb2 O1 84.19(16) . 11_556 ? O5 Tb2 O1 138.88(7) . 11_556 ? O1 Tb2 O1 69.43(11) . 11_556 ? O1 Tb2 O1 69.43(11) 8_645 11_556 ? O2 Tb2 C2B 150.8(2) 8_645 19_564 ? O2 Tb2 C2B 59.2(2) 11_556 19_564 ? O2 Tb2 C2B 56.8(3) . 19_564 ? O5 Tb2 C2B 73.4(2) . 19_564 ? O1 Tb2 C2B 119.2(2) . 19_564 ? O1 Tb2 C2B 65.6(2) 8_645 19_564 ? O1 Tb2 C2B 124.8(2) 11_556 19_564 ? O2 Tb2 O4B 150.8(2) 8_645 19_564 ? O2 Tb2 O4B 59.2(2) 11_556 19_564 ? O2 Tb2 O4B 56.8(3) . 19_564 ? O5 Tb2 O4B 73.4(2) . 19_564 ? O1 Tb2 O4B 119.2(2) . 19_564 ? O1 Tb2 O4B 65.6(2) 8_645 19_564 ? O1 Tb2 O4B 124.8(2) 11_556 19_564 ? C2B Tb2 O4B 0.0(4) 19_564 19_564 ? O2 Tb2 C2B 59.2(2) 8_645 14_654 ? O2 Tb2 C2B 56.8(3) 11_556 14_654 ? O2 Tb2 C2B 150.8(2) . 14_654 ? O5 Tb2 C2B 73.4(2) . 14_654 ? O1 Tb2 C2B 65.6(2) . 14_654 ? O1 Tb2 C2B 124.8(2) 8_645 14_654 ? O1 Tb2 C2B 119.2(2) 11_556 14_654 ? C2B Tb2 C2B 112.17(18) 19_564 14_654 ? O4B Tb2 C2B 112.17(18) 19_564 14_654 ? O2 Tb2 O4B 59.2(2) 8_645 14_654 ? O2 Tb2 O4B 56.8(3) 11_556 14_654 ? O2 Tb2 O4B 150.8(2) . 14_654 ? O5 Tb2 O4B 73.4(2) . 14_654 ? O1 Tb2 O4B 65.6(2) . 14_654 ? O1 Tb2 O4B 124.8(2) 8_645 14_654 ? O1 Tb2 O4B 119.2(2) 11_556 14_654 ? C2B Tb2 O4B 112.17(18) 19_564 14_654 ? O4B Tb2 O4B 112.17(18) 19_564 14_654 ? C2B Tb2 O4B 0.0(5) 14_654 14_654 ? O2 Tb2 C2B 56.8(3) 8_645 24_553 ? O2 Tb2 C2B 150.8(2) 11_556 24_553 ? O2 Tb2 C2B 59.2(2) . 24_553 ? O5 Tb2 C2B 73.4(2) . 24_553 ? O1 Tb2 C2B 124.8(2) . 24_553 ? O1 Tb2 C2B 119.2(2) 8_645 24_553 ? O1 Tb2 C2B 65.6(2) 11_556 24_553 ? C2B Tb2 C2B 112.17(18) 19_564 24_553 ? O4B Tb2 C2B 112.17(18) 19_564 24_553 ? C2B Tb2 C2B 112.17(18) 14_654 24_553 ? O4B Tb2 C2B 112.17(18) 14_654 24_553 ? O3 P1 O2 112.5(2) 24_553 22_645 ? O3 P1 O1 111.25(18) 24_553 . ? O2 P1 O1 111.6(3) 22_645 . ? O3 P1 C1 107.6(2) 24_553 . ? O2 P1 C1 107.5(2) 22_645 . ? O1 P1 C1 106.04(18) . . ? P1 O1 Tb1 132.11(18) . . ? P1 O1 Tb2 132.34(18) . . ? Tb1 O1 Tb2 95.46(10) . . ? P1 O2 Tb2 135.5(3) 19_564 . ? P1 O3 Tb1 149.6(2) 18 . ? C2A O4A O4A 0.0(16) 14_654 14_654 ? C2A O4A C1 67.4(6) 14_654 . ? O4A O4A C1 67.4(6) 14_654 . ? C1 O4B Tb2 109.8(5) . 14_654 ? O4A C1 C2A 45.1(12) . 14_654 ? O4A C1 O4A 45.1(12) . 14_654 ? C2A C1 O4A 0.0(13) 14_654 14_654 ? O4A C1 O4B 102.2(8) . . ? C2A C1 O4B 60.7(8) 14_654 . ? O4A C1 O4B 60.7(8) 14_654 . ? O4A C1 C2B 60.7(8) . 14_654 ? C2A C1 C2B 102.2(8) 14_654 14_654 ? O4A C1 C2B 102.2(8) 14_654 14_654 ? O4B C1 C2B 162.6(9) . 14_654 ? O4A C1 O4B 60.7(8) . 14_654 ? C2A C1 O4B 102.2(8) 14_654 14_654 ? O4A C1 O4B 102.2(8) 14_654 14_654 ? O4B C1 O4B 162.6(9) . 14_654 ? C2B C1 O4B 0.0(10) 14_654 14_654 ? O4A C1 P1 127.6(7) . 14_654 ? C2A C1 P1 115.5(6) 14_654 14_654 ? O4A C1 P1 115.5(6) 14_654 14_654 ? O4B C1 P1 99.9(4) . 14_654 ? C2B C1 P1 89.9(4) 14_654 14_654 ? O4B C1 P1 89.9(4) 14_654 14_654 ? O4A C1 P1 115.5(6) . . ? C2A C1 P1 127.6(7) 14_654 . ? O4A C1 P1 127.6(7) 14_654 . ? O4B C1 P1 89.9(4) . . ? C2B C1 P1 99.9(4) 14_654 . ? O4B C1 P1 99.9(4) 14_654 . ? P1 C1 P1 111.4(4) 14_654 . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 36.27 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.097 _refine_diff_density_min -1.717 _refine_diff_density_rms 0.186 _database_code_depnum_ccdc_archive 'CCDC 934837' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_publication_text _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H8 O11.50 P3 Y2' _chemical_formula_weight 498.82 _chemical_absolute_configuration unk 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M I2(1)3 _symmetry_space_group_name_Hall 'I 2b 2c 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-x+1/2, y+1, -z+1' 'x+1, -y+1, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1, -x+1, -y+1/2' '-z+1, -x+1/2, y+1' '-z+1/2, x+1, -y+1' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1, -x+1' 'y+1, -z+1, -x+1/2' '-y+1, -z+1/2, x+1' _cell_length_a 13.4853(2) _cell_length_b 13.4853(2) _cell_length_c 13.4853(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2452.35(6) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2964 _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 25.86 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.702 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 9.866 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2697 _exptl_absorpt_correction_T_max 0.3388 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7856 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.16 _reflns_number_total 912 _reflns_number_gt 833 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0359P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.035(11) _refine_ls_number_reflns 912 _refine_ls_number_parameters 70 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0306 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0628 _refine_ls_wR_factor_gt 0.0620 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.000 _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 Y1 Y 0.92798(3) 0.42798(3) 0.07202(3) 0.01352(17) Uani 1 3 d S . . Y2 Y 0.77848(3) 0.27848(3) 0.22152(3) 0.01797(19) Uani 1 3 d S . . P1 P 1.02094(9) 0.35874(9) 0.30511(9) 0.0217(3) Uani 1 1 d . . . O1 O 0.9386(2) 0.3578(2) 0.2270(2) 0.0220(7) Uani 1 1 d . . . O2 O 1.1216(3) 0.3471(3) 0.2606(3) 0.0442(12) Uani 1 1 d . . . O3 O 0.8706(2) 0.5130(3) -0.0523(3) 0.0289(8) Uani 1 1 d . . . O4A O 1.054(2) 0.2339(8) 0.4690(11) 0.098(12) Uani 0.236(11) 1 d P . 1 C2A C 1.054(2) 0.2339(8) 0.4690(11) 0.098(12) Uani 0.236(11) 1 d P . 1 O4B O 1.1246(7) 0.2356(7) 0.4043(11) 0.044(4) Uani 0.264(11) 1 d P . 2 C2B C 1.1246(7) 0.2356(7) 0.4043(11) 0.044(4) Uani 0.264(11) 1 d P . 2 O5 O 0.6757(3) 0.1757(3) 0.3243(3) 0.056(2) Uani 1 3 d S . . C1 C 1.0000 0.2500 0.3816(6) 0.052(3) Uani 1 2 d S . . 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 Y1 0.01352(17) 0.01352(17) 0.01352(17) -0.00092(17) -0.00092(17) 0.00092(17) Y2 0.01797(19) 0.01797(19) 0.01797(19) 0.00049(18) 0.00049(18) -0.00049(18) P1 0.0214(6) 0.0229(6) 0.0208(6) -0.0066(5) -0.0053(5) 0.0061(5) O1 0.0264(17) 0.0205(15) 0.0190(16) 0.0001(14) -0.0063(15) -0.0002(14) O2 0.0224(18) 0.033(2) 0.077(3) -0.032(2) 0.006(2) -0.0004(16) O3 0.0263(18) 0.033(2) 0.028(2) 0.0126(16) -0.0079(16) -0.0091(16) O4A 0.22(3) 0.036(7) 0.037(9) -0.008(6) -0.075(14) 0.027(10) C2A 0.22(3) 0.036(7) 0.037(9) -0.008(6) -0.075(14) 0.027(10) O4B 0.026(5) 0.045(6) 0.061(9) -0.011(5) -0.020(5) 0.004(4) C2B 0.026(5) 0.045(6) 0.061(9) -0.011(5) -0.020(5) 0.004(4) O5 0.056(2) 0.056(2) 0.056(2) 0.0200(18) 0.0200(18) -0.0200(18) C1 0.112(9) 0.024(4) 0.021(4) 0.000 0.000 0.021(5) _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 Y1 O3 2.173(3) 11_556 ? Y1 O3 2.173(3) 8_645 ? Y1 O3 2.173(3) . ? Y1 O1 2.299(3) 11_556 ? Y1 O1 2.299(3) 8_645 ? Y1 O1 2.299(3) . ? Y1 Y2 3.4919(10) . ? Y2 O2 2.227(4) 24_553 ? Y2 O2 2.227(4) 19_564 ? Y2 O2 2.227(4) 14_654 ? Y2 O5 2.401(7) . ? Y2 O1 2.411(3) . ? Y2 O1 2.411(3) 11_556 ? Y2 O1 2.411(3) 8_645 ? Y2 C2B 2.796(15) 24_553 ? Y2 O4B 2.796(15) 24_553 ? Y2 C2B 2.796(15) 14_654 ? Y2 O4B 2.796(15) 14_654 ? Y2 C2B 2.796(15) 19_564 ? P1 O2 1.492(4) . ? P1 O3 1.494(3) 21_554 ? P1 O1 1.530(3) . ? P1 C1 1.815(5) . ? O2 Y2 2.227(4) 14_654 ? O3 P1 1.494(3) 17_544 ? O4A C1 1.403(12) . ? O4A C2A 1.52(5) 14_654 ? O4A O4A 1.52(5) 14_654 ? O4B C1 1.719(8) . ? O4B Y2 2.796(15) 14_654 ? C1 C2A 1.403(12) 14_654 ? C1 O4A 1.403(12) 14_654 ? C1 C2B 1.719(8) 14_654 ? C1 O4B 1.719(8) 14_654 ? C1 P1 1.815(5) 14_654 ? 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 Y1 O3 93.16(11) 11_556 8_645 ? O3 Y1 O3 93.16(11) 11_556 . ? O3 Y1 O3 93.16(11) 8_645 . ? O3 Y1 O1 160.20(12) 11_556 11_556 ? O3 Y1 O1 87.79(12) 8_645 11_556 ? O3 Y1 O1 106.53(12) . 11_556 ? O3 Y1 O1 106.54(12) 11_556 8_645 ? O3 Y1 O1 160.20(12) 8_645 8_645 ? O3 Y1 O1 87.79(12) . 8_645 ? O1 Y1 O1 73.04(13) 11_556 8_645 ? O3 Y1 O1 87.79(12) 11_556 . ? O3 Y1 O1 106.54(12) 8_645 . ? O3 Y1 O1 160.20(12) . . ? O1 Y1 O1 73.04(13) 11_556 . ? O1 Y1 O1 73.04(13) 8_645 . ? O3 Y1 Y2 122.99(8) 11_556 . ? O3 Y1 Y2 122.99(8) 8_645 . ? O3 Y1 Y2 122.99(8) . . ? O1 Y1 Y2 43.40(8) 11_556 . ? O1 Y1 Y2 43.40(8) 8_645 . ? O1 Y1 Y2 43.40(8) . . ? O2 Y2 O2 115.05(7) 24_553 19_564 ? O2 Y2 O2 115.05(7) 24_553 14_654 ? O2 Y2 O2 115.05(7) 19_564 14_654 ? O2 Y2 O5 76.94(9) 24_553 . ? O2 Y2 O5 76.94(9) 19_564 . ? O2 Y2 O5 76.94(9) 14_654 . ? O2 Y2 O1 143.55(12) 24_553 . ? O2 Y2 O1 85.42(13) 19_564 . ? O2 Y2 O1 77.75(12) 14_654 . ? O5 Y2 O1 139.07(8) . . ? O2 Y2 O1 77.75(12) 24_553 11_556 ? O2 Y2 O1 143.54(12) 19_564 11_556 ? O2 Y2 O1 85.42(13) 14_654 11_556 ? O5 Y2 O1 139.07(8) . 11_556 ? O1 Y2 O1 69.13(12) . 11_556 ? O2 Y2 O1 85.42(13) 24_553 8_645 ? O2 Y2 O1 77.75(12) 19_564 8_645 ? O2 Y2 O1 143.54(12) 14_654 8_645 ? O5 Y2 O1 139.07(8) . 8_645 ? O1 Y2 O1 69.13(12) . 8_645 ? O1 Y2 O1 69.13(12) 11_556 8_645 ? O2 Y2 C2B 57.1(2) 24_553 24_553 ? O2 Y2 C2B 150.8(2) 19_564 24_553 ? O2 Y2 C2B 58.8(2) 14_654 24_553 ? O5 Y2 C2B 73.83(18) . 24_553 ? O1 Y2 C2B 117.8(2) . 24_553 ? O1 Y2 C2B 65.5(2) 11_556 24_553 ? O1 Y2 C2B 125.48(17) 8_645 24_553 ? O2 Y2 O4B 57.1(2) 24_553 24_553 ? O2 Y2 O4B 150.8(2) 19_564 24_553 ? O2 Y2 O4B 58.8(2) 14_654 24_553 ? O5 Y2 O4B 73.83(18) . 24_553 ? O1 Y2 O4B 117.8(2) . 24_553 ? O1 Y2 O4B 65.5(2) 11_556 24_553 ? O1 Y2 O4B 125.48(17) 8_645 24_553 ? C2B Y2 O4B 0.0(6) 24_553 24_553 ? O2 Y2 C2B 150.8(2) 24_553 14_654 ? O2 Y2 C2B 58.8(2) 19_564 14_654 ? O2 Y2 C2B 57.1(2) 14_654 14_654 ? O5 Y2 C2B 73.83(18) . 14_654 ? O1 Y2 C2B 65.5(2) . 14_654 ? O1 Y2 C2B 125.48(18) 11_556 14_654 ? O1 Y2 C2B 117.8(2) 8_645 14_654 ? C2B Y2 C2B 112.56(15) 24_553 14_654 ? O4B Y2 C2B 112.56(15) 24_553 14_654 ? O2 Y2 O4B 150.8(2) 24_553 14_654 ? O2 Y2 O4B 58.8(2) 19_564 14_654 ? O2 Y2 O4B 57.1(2) 14_654 14_654 ? O5 Y2 O4B 73.83(18) . 14_654 ? O1 Y2 O4B 65.5(2) . 14_654 ? O1 Y2 O4B 125.48(18) 11_556 14_654 ? O1 Y2 O4B 117.8(2) 8_645 14_654 ? C2B Y2 O4B 112.56(15) 24_553 14_654 ? O4B Y2 O4B 112.56(15) 24_553 14_654 ? C2B Y2 O4B 0.0(5) 14_654 14_654 ? O2 Y2 C2B 58.8(2) 24_553 19_564 ? O2 Y2 C2B 57.1(2) 19_564 19_564 ? O2 Y2 C2B 150.8(2) 14_654 19_564 ? O5 Y2 C2B 73.83(18) . 19_564 ? O1 Y2 C2B 125.48(18) . 19_564 ? O1 Y2 C2B 117.8(2) 11_556 19_564 ? O1 Y2 C2B 65.5(2) 8_645 19_564 ? C2B Y2 C2B 112.56(15) 24_553 19_564 ? O4B Y2 C2B 112.56(15) 24_553 19_564 ? C2B Y2 C2B 112.56(15) 14_654 19_564 ? O4B Y2 C2B 112.56(15) 14_654 19_564 ? O2 P1 O3 112.8(2) . 21_554 ? O2 P1 O1 112.4(2) . . ? O3 P1 O1 111.23(19) 21_554 . ? O2 P1 C1 106.57(19) . . ? O3 P1 C1 107.5(2) 21_554 . ? O1 P1 C1 105.76(19) . . ? P1 O1 Y1 131.89(18) . . ? P1 O1 Y2 132.41(18) . . ? Y1 O1 Y2 95.67(12) . . ? P1 O2 Y2 136.5(2) . 14_654 ? P1 O3 Y1 150.2(2) 17_544 . ? C1 O4A C2A 57.1(12) . 14_654 ? C1 O4A O4A 57.1(12) . 14_654 ? C2A O4A O4A 0.0(16) 14_654 14_654 ? C1 O4B Y2 107.9(6) . 14_654 ? O4A C1 C2A 66(2) . 14_654 ? O4A C1 O4A 66(2) . 14_654 ? C2A C1 O4A 0(2) 14_654 14_654 ? O4A C1 C2B 112.2(17) . 14_654 ? C2A C1 C2B 47.5(10) 14_654 14_654 ? O4A C1 C2B 47.5(10) 14_654 14_654 ? O4A C1 O4B 112.2(17) . 14_654 ? C2A C1 O4B 47.5(10) 14_654 14_654 ? O4A C1 O4B 47.5(10) 14_654 14_654 ? C2B C1 O4B 0.0(9) 14_654 14_654 ? O4A C1 O4B 47.5(10) . . ? C2A C1 O4B 112.2(17) 14_654 . ? O4A C1 O4B 112.2(17) 14_654 . ? C2B C1 O4B 159.5(11) 14_654 . ? O4B C1 O4B 159.5(11) 14_654 . ? O4A C1 P1 115.7(5) . 14_654 ? C2A C1 P1 121.4(8) 14_654 14_654 ? O4A C1 P1 121.4(8) 14_654 14_654 ? C2B C1 P1 92.3(4) 14_654 14_654 ? O4B C1 P1 92.3(4) 14_654 14_654 ? O4B C1 P1 99.3(4) . 14_654 ? O4A C1 P1 121.4(8) . . ? C2A C1 P1 115.7(5) 14_654 . ? O4A C1 P1 115.7(5) 14_654 . ? C2B C1 P1 99.3(4) 14_654 . ? O4B C1 P1 99.3(4) 14_654 . ? O4B C1 P1 92.3(4) . . ? P1 C1 P1 110.7(4) 14_654 . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.16 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.468 _refine_diff_density_min -0.394 _refine_diff_density_rms 0.097 _database_code_depnum_ccdc_archive 'CCDC 934838' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_publication_text _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H8 Er2 O11.50 P3' _chemical_formula_weight 655.52 _chemical_absolute_configuration unk 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M I2(1)3 _symmetry_space_group_name_Hall 'I 2b 2c 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-x+1/2, y+1, -z+1' 'x+1, -y+1, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1, -x+1, -y+1/2' '-z+1, -x+1/2, y+1' '-z+1/2, x+1, -y+1' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1, -x+1' 'y+1, -z+1, -x+1/2' '-y+1, -z+1/2, x+1' _cell_length_a 13.52000(10) _cell_length_b 13.52000(10) _cell_length_c 13.52000(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2471.33(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9977 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 41.44 _exptl_crystal_description cubic _exptl_crystal_colour pink _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2392 _exptl_absorpt_coefficient_mu 13.934 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1882 _exptl_absorpt_correction_T_max 0.2140 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19790 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0276 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.69 _diffrn_reflns_theta_max 40.16 _reflns_number_total 2476 _reflns_number_gt 2339 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Me/OH disorder was refined by part instruction and restrained via EADP and EXYZ commands. No hydrogen atom added because of the disorder. EADP O4b C2b EXYZ O4b C2b EADP O4a C2a EXYZ O4a C2a part 1 O4A 3 0.644148 0.512772 0.119309 20.50000 0.06667 0.04293 = 0.06777 0.00153 0.00761 -0.00823 part 2 O4B 3 0.728029 0.517397 0.227679 -20.50000 0.03314 0.09763 = 0.07647 0.01702 0.00881 0.03727 part 0 part 1 C2A 1 0.644148 0.512772 0.119309 20.50000 0.06667 0.04293 = 0.06777 0.00153 0.00761 -0.00823 part 2 C2B 1 0.728029 0.517397 0.227679 -20.50000 0.03314 0.09763 = 0.07647 0.01702 0.00881 0.03727 part 0 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^)+(0.0368P)^2^+22.9333P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(2) _refine_ls_number_reflns 2476 _refine_ls_number_parameters 70 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0349 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0821 _refine_ls_wR_factor_gt 0.0808 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_restrained_S_all 1.159 _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 Er1 Er 0.320736(13) 0.679264(13) 0.179264(13) 0.00992(6) Uani 1 3 d S . . Er2 Er 0.470117(16) 0.529883(16) 0.029883(16) 0.01768(8) Uani 1 3 d S . . P1 P 0.55376(10) 0.60884(10) 0.27136(9) 0.0146(2) Uani 1 1 d . . . O1 O 0.4760(3) 0.6087(3) 0.1894(3) 0.0177(6) Uani 1 1 d . . . O2 O 0.5068(6) 0.4025(4) 0.1265(3) 0.0451(17) Uani 1 1 d . . . O3 O 0.1975(3) 0.7638(4) 0.1203(3) 0.0238(8) Uani 1 1 d . . . O4A O 0.6441(14) 0.5128(13) 0.1193(15) 0.059(5) Uani 0.277(11) 1 d P . 1 O4B O 0.7280(12) 0.517(2) 0.2277(19) 0.069(9) Uani 0.223(11) 1 d P . 2 O5 O 0.5720(4) 0.4280(4) -0.0720(4) 0.047(3) Uani 1 3 d S . . C1 C 0.6265(7) 0.5000 0.2500 0.041(3) Uani 1 2 d S . . C2A C 0.6441(14) 0.5128(13) 0.1193(15) 0.059(5) Uani 0.277(11) 1 d P . 1 C2B C 0.7280(12) 0.517(2) 0.2277(19) 0.069(9) Uani 0.223(11) 1 d P . 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 Er1 0.00992(6) 0.00992(6) 0.00992(6) 0.00078(6) -0.00078(6) -0.00078(6) Er2 0.01768(8) 0.01768(8) 0.01768(8) -0.00126(7) 0.00126(7) 0.00126(7) P1 0.0147(5) 0.0142(5) 0.0148(5) 0.0046(4) -0.0039(4) -0.0051(4) O1 0.0173(14) 0.0134(12) 0.0224(16) -0.0011(12) -0.0091(13) 0.0016(11) O2 0.088(5) 0.029(2) 0.0180(18) -0.0006(17) -0.011(2) 0.030(3) O3 0.0210(17) 0.0279(19) 0.0226(17) -0.0088(15) -0.0103(14) 0.0113(15) O4A 0.067(11) 0.043(8) 0.068(11) 0.002(7) 0.008(8) -0.008(8) O4B 0.033(8) 0.10(2) 0.076(19) 0.017(13) 0.009(8) 0.037(10) O5 0.047(3) 0.047(3) 0.047(3) -0.016(2) 0.016(2) 0.016(2) C1 0.017(3) 0.019(3) 0.086(9) 0.024(5) 0.000 0.000 C2A 0.067(11) 0.043(8) 0.068(11) 0.002(7) 0.008(8) -0.008(8) C2B 0.033(8) 0.10(2) 0.076(19) 0.017(13) 0.009(8) 0.037(10) _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 Er1 O3 2.172(4) 7_564 ? Er1 O3 2.172(4) 10_655 ? Er1 O3 2.172(4) . ? Er1 O1 2.310(4) . ? Er1 O1 2.310(4) 7_564 ? Er1 O1 2.310(4) 10_655 ? Er1 Er2 3.4981(5) . ? Er2 O2 2.218(5) . ? Er2 O2 2.218(5) 7_564 ? Er2 O2 2.218(5) 10_655 ? Er2 O5 2.385(10) . ? Er2 O1 2.407(4) 7_564 ? Er2 O1 2.407(4) 10_655 ? Er2 O1 2.407(4) . ? Er2 C2A 2.66(2) 7_564 ? Er2 O4A 2.66(2) 7_564 ? Er2 C2A 2.66(2) 10_655 ? Er2 O4A 2.66(2) 10_655 ? P1 O3 1.503(4) 17_554 ? P1 O1 1.527(4) . ? P1 O2 1.528(5) 16_455 ? P1 C1 1.793(5) . ? O2 P1 1.528(5) 16_455 ? O3 P1 1.502(4) 21_454 ? O4A C1 1.79(2) . ? O4B C2B 0.77(4) 16_455 ? O4B O4B 0.77(4) 16_455 ? O4B C1 1.43(2) . ? C1 C2B 1.43(2) 16_455 ? C1 O4B 1.43(2) 16_455 ? C1 C2A 1.79(2) 16_455 ? C1 O4A 1.79(2) 16_455 ? C1 P1 1.793(5) 16_455 ? 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 Er1 O3 94.08(15) 7_564 10_655 ? O3 Er1 O3 94.08(15) 7_564 . ? O3 Er1 O3 94.08(15) 10_655 . ? O3 Er1 O1 87.23(15) 7_564 . ? O3 Er1 O1 106.35(16) 10_655 . ? O3 Er1 O1 159.40(17) . . ? O3 Er1 O1 159.40(17) 7_564 7_564 ? O3 Er1 O1 87.23(15) 10_655 7_564 ? O3 Er1 O1 106.35(16) . 7_564 ? O1 Er1 O1 72.73(15) . 7_564 ? O3 Er1 O1 106.35(16) 7_564 10_655 ? O3 Er1 O1 159.40(17) 10_655 10_655 ? O3 Er1 O1 87.23(15) . 10_655 ? O1 Er1 O1 72.73(15) . 10_655 ? O1 Er1 O1 72.73(15) 7_564 10_655 ? O3 Er1 Er2 122.32(11) 7_564 . ? O3 Er1 Er2 122.32(11) 10_655 . ? O3 Er1 Er2 122.32(11) . . ? O1 Er1 Er2 43.21(9) . . ? O1 Er1 Er2 43.21(9) 7_564 . ? O1 Er1 Er2 43.21(9) 10_655 . ? O2 Er2 O2 114.55(11) . 7_564 ? O2 Er2 O2 114.56(11) . 10_655 ? O2 Er2 O2 114.55(11) 7_564 10_655 ? O2 Er2 O5 76.27(15) . . ? O2 Er2 O5 76.27(15) 7_564 . ? O2 Er2 O5 76.27(15) 10_655 . ? O2 Er2 O1 85.0(2) . 7_564 ? O2 Er2 O1 78.97(15) 7_564 7_564 ? O2 Er2 O1 144.52(17) 10_655 7_564 ? O5 Er2 O1 138.92(9) . 7_564 ? O2 Er2 O1 144.52(17) . 10_655 ? O2 Er2 O1 85.0(2) 7_564 10_655 ? O2 Er2 O1 78.97(15) 10_655 10_655 ? O5 Er2 O1 138.92(9) . 10_655 ? O1 Er2 O1 69.37(14) 7_564 10_655 ? O2 Er2 O1 78.97(15) . . ? O2 Er2 O1 144.52(17) 7_564 . ? O2 Er2 O1 85.0(2) 10_655 . ? O5 Er2 O1 138.92(9) . . ? O1 Er2 O1 69.37(14) 7_564 . ? O1 Er2 O1 69.37(14) 10_655 . ? O2 Er2 C2A 57.7(4) . 7_564 ? O2 Er2 C2A 57.7(4) 7_564 7_564 ? O2 Er2 C2A 148.9(4) 10_655 7_564 ? O5 Er2 C2A 72.6(4) . 7_564 ? O1 Er2 C2A 66.5(4) 7_564 7_564 ? O1 Er2 C2A 126.1(4) 10_655 7_564 ? O1 Er2 C2A 119.1(4) . 7_564 ? O2 Er2 O4A 57.7(4) . 7_564 ? O2 Er2 O4A 57.7(4) 7_564 7_564 ? O2 Er2 O4A 148.9(4) 10_655 7_564 ? O5 Er2 O4A 72.6(4) . 7_564 ? O1 Er2 O4A 66.5(4) 7_564 7_564 ? O1 Er2 O4A 126.1(4) 10_655 7_564 ? O1 Er2 O4A 119.1(4) . 7_564 ? C2A Er2 O4A 0.0(11) 7_564 7_564 ? O2 Er2 C2A 148.9(4) . 10_655 ? O2 Er2 C2A 57.7(4) 7_564 10_655 ? O2 Er2 C2A 57.7(4) 10_655 10_655 ? O5 Er2 C2A 72.6(4) . 10_655 ? O1 Er2 C2A 119.1(4) 7_564 10_655 ? O1 Er2 C2A 66.5(4) 10_655 10_655 ? O1 Er2 C2A 126.1(4) . 10_655 ? C2A Er2 C2A 111.5(4) 7_564 10_655 ? O4A Er2 C2A 111.5(4) 7_564 10_655 ? O2 Er2 O4A 148.9(4) . 10_655 ? O2 Er2 O4A 57.7(4) 7_564 10_655 ? O2 Er2 O4A 57.7(4) 10_655 10_655 ? O5 Er2 O4A 72.6(4) . 10_655 ? O1 Er2 O4A 119.1(4) 7_564 10_655 ? O1 Er2 O4A 66.5(4) 10_655 10_655 ? O1 Er2 O4A 126.1(4) . 10_655 ? C2A Er2 O4A 111.5(4) 7_564 10_655 ? O4A Er2 O4A 111.5(4) 7_564 10_655 ? C2A Er2 O4A 0.0(9) 10_655 10_655 ? O3 P1 O1 111.3(2) 17_554 . ? O3 P1 O2 113.0(3) 17_554 16_455 ? O1 P1 O2 111.7(4) . 16_455 ? O3 P1 C1 108.4(3) 17_554 . ? O1 P1 C1 105.1(2) . . ? O2 P1 C1 106.9(3) 16_455 . ? P1 O1 Er1 131.9(2) . . ? P1 O1 Er2 132.3(2) . . ? Er1 O1 Er2 95.71(13) . . ? P1 O2 Er2 134.7(4) 16_455 . ? P1 O3 Er1 150.2(3) 21_454 . ? C1 O4A Er2 109.8(9) . . ? C2B O4B O4B 0(4) 16_455 16_455 ? C2B O4B C1 74.4(8) 16_455 . ? O4B O4B C1 74.4(8) 16_455 . ? O4B C1 C2B 31.1(17) . 16_455 ? O4B C1 O4B 31.1(17) . 16_455 ? C2B C1 O4B 0(2) 16_455 16_455 ? O4B C1 C2A 95.5(13) . 16_455 ? C2B C1 C2A 69.3(12) 16_455 16_455 ? O4B C1 C2A 69.3(12) 16_455 16_455 ? O4B C1 O4A 95.5(13) . 16_455 ? C2B C1 O4A 69.3(12) 16_455 16_455 ? O4B C1 O4A 69.3(12) 16_455 16_455 ? C2A C1 O4A 0.0(11) 16_455 16_455 ? O4B C1 O4A 69.3(12) . . ? C2B C1 O4A 95.5(13) 16_455 . ? O4B C1 O4A 95.5(13) 16_455 . ? C2A C1 O4A 164.7(14) 16_455 . ? O4A C1 O4A 164.7(14) 16_455 . ? O4B C1 P1 129.0(13) . 16_455 ? C2B C1 P1 115.3(12) 16_455 16_455 ? O4B C1 P1 115.3(12) 16_455 16_455 ? C2A C1 P1 98.8(6) 16_455 16_455 ? O4A C1 P1 98.8(6) 16_455 16_455 ? O4A C1 P1 89.6(6) . 16_455 ? O4B C1 P1 115.3(12) . . ? C2B C1 P1 129.0(13) 16_455 . ? O4B C1 P1 129.0(13) 16_455 . ? C2A C1 P1 89.6(6) 16_455 . ? O4A C1 P1 89.6(6) 16_455 . ? O4A C1 P1 98.8(6) . . ? P1 C1 P1 113.5(5) 16_455 . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 40.16 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.966 _refine_diff_density_min -3.742 _refine_diff_density_rms 0.287 _database_code_depnum_ccdc_archive 'CCDC 948279' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_yp380 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H2 O11.50 P3 Y2' _chemical_formula_weight 456.75 _chemical_absolute_configuration unk loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M I2(1)3 _symmetry_space_group_name_Hall 'I 2b 2c 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-x+1/2, y+1, -z+1' 'x+1, -y+1, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1, -x+1, -y+1/2' '-z+1, -x+1/2, y+1' '-z+1/2, x+1, -y+1' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1, -x+1' 'y+1, -z+1, -x+1/2' '-y+1, -z+1/2, x+1' _cell_length_a 13.3727(4) _cell_length_b 13.3727(4) _cell_length_c 13.3727(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2391.43(12) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 695 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 21.25 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 10.104 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2635 _exptl_absorpt_correction_T_max 0.3769 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 2755 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0613 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 25.27 _reflns_number_total 722 _reflns_number_gt 553 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(4) _refine_ls_number_reflns 722 _refine_ls_number_parameters 52 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1021 _refine_ls_R_factor_gt 0.0792 _refine_ls_wR_factor_ref 0.2129 _refine_ls_wR_factor_gt 0.1941 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.127 _refine_ls_shift/su_max 0.000 _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 Y1 Y 0.06375(10) 0.56375(10) 0.93625(10) 0.0349(7) Uani 1 3 d S . . Y2 Y 0.21906(16) 0.71906(16) 0.78094(16) 0.0692(12) Uani 1 3 d S . . P1 P 0.1437(3) 0.8021(3) 1.0237(3) 0.0473(12) Uani 1 1 d . . . O1 O 0.1358(9) 0.7192(10) 0.9476(12) 0.068(4) Uani 1 1 d . . . O2 O 0.1395(15) 0.7621(16) 1.1239(12) 0.104(6) Uani 1 1 d . . . O3 O 0.1205(10) 0.4920(12) 1.0664(12) 0.074(4) Uani 1 1 d . . . O4 O 0.2500 0.8543(13) 1.0000 0.075(5) Uani 1 2 d SU . . O5 O 0.3169(7) 0.8169(7) 0.6831(7) 0.048(5) Uani 1 3 d S . . 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 Y1 0.0349(7) 0.0349(7) 0.0349(7) 0.0001(6) 0.0001(6) -0.0001(6) Y2 0.0692(12) 0.0692(12) 0.0692(12) 0.0004(9) 0.0004(9) -0.0004(9) P1 0.034(2) 0.043(2) 0.065(3) -0.011(2) -0.0154(18) 0.0091(19) O1 0.038(6) 0.061(7) 0.104(10) -0.029(7) -0.018(6) -0.007(5) O2 0.130(16) 0.115(14) 0.069(10) 0.014(10) 0.009(10) -0.020(13) O3 0.079(9) 0.082(9) 0.063(8) 0.013(8) -0.025(7) -0.015(8) O4 0.036(8) 0.049(9) 0.140(14) 0.000 -0.021(9) 0.000 O5 0.048(5) 0.048(5) 0.048(5) 0.016(4) 0.016(4) -0.016(4) _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 Y1 O3 2.128(15) . ? Y1 O3 2.128(15) 11_466 ? Y1 O3 2.128(15) 8_656 ? Y1 O1 2.296(12) . ? Y1 O1 2.296(12) 8_656 ? Y1 O1 2.296(12) 11_466 ? Y1 Y2 3.597(5) . ? Y2 O5 2.267(16) . ? Y2 O2 2.35(2) 21_445 ? Y2 O2 2.35(2) 18_356 ? Y2 O2 2.35(2) 15_546 ? Y2 O1 2.492(16) . ? Y2 O1 2.492(16) 8_656 ? Y2 O1 2.492(16) 11_466 ? P1 O2 1.444(18) . ? P1 O3 1.477(14) 18_356 ? P1 O1 1.508(13) . ? P1 O4 1.615(9) . ? O2 Y2 2.35(2) 15_546 ? O3 P1 1.477(14) 24_565 ? O4 P1 1.615(9) 15_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 O3 Y1 O3 94.8(5) . 11_466 ? O3 Y1 O3 94.8(5) . 8_656 ? O3 Y1 O3 94.8(5) 11_466 8_656 ? O3 Y1 O1 101.8(6) . . ? O3 Y1 O1 162.4(6) 11_466 . ? O3 Y1 O1 89.4(6) 8_656 . ? O3 Y1 O1 162.4(6) . 8_656 ? O3 Y1 O1 89.4(5) 11_466 8_656 ? O3 Y1 O1 101.8(6) 8_656 8_656 ? O1 Y1 O1 73.0(6) . 8_656 ? O3 Y1 O1 89.4(6) . 11_466 ? O3 Y1 O1 101.8(6) 11_466 11_466 ? O3 Y1 O1 162.5(6) 8_656 11_466 ? O1 Y1 O1 73.0(6) . 11_466 ? O1 Y1 O1 73.0(6) 8_656 11_466 ? O3 Y1 Y2 121.8(4) . . ? O3 Y1 Y2 121.8(4) 11_466 . ? O3 Y1 Y2 121.8(4) 8_656 . ? O1 Y1 Y2 43.4(4) . . ? O1 Y1 Y2 43.4(4) 8_656 . ? O1 Y1 Y2 43.4(4) 11_466 . ? O5 Y2 O2 72.9(5) . 21_445 ? O5 Y2 O2 72.9(5) . 18_356 ? O2 Y2 O2 111.8(4) 21_445 18_356 ? O5 Y2 O2 72.9(5) . 15_546 ? O2 Y2 O2 111.8(4) 21_445 15_546 ? O2 Y2 O2 111.8(4) 18_356 15_546 ? O5 Y2 O1 140.7(3) . . ? O2 Y2 O1 146.1(5) 21_445 . ? O2 Y2 O1 88.7(6) 18_356 . ? O2 Y2 O1 82.8(5) 15_546 . ? O5 Y2 O1 140.7(3) . 8_656 ? O2 Y2 O1 88.7(6) 21_445 8_656 ? O2 Y2 O1 82.8(5) 18_356 8_656 ? O2 Y2 O1 146.1(5) 15_546 8_656 ? O1 Y2 O1 66.5(4) . 8_656 ? O5 Y2 O1 140.7(3) . 11_466 ? O2 Y2 O1 82.8(5) 21_445 11_466 ? O2 Y2 O1 146.1(6) 18_356 11_466 ? O2 Y2 O1 88.7(6) 15_546 11_466 ? O1 Y2 O1 66.5(4) . 11_466 ? O1 Y2 O1 66.5(4) 8_656 11_466 ? O5 Y2 Y1 180.0(3) . . ? O2 Y2 Y1 107.1(5) 21_445 . ? O2 Y2 Y1 107.1(5) 18_356 . ? O2 Y2 Y1 107.1(5) 15_546 . ? O1 Y2 Y1 39.3(3) . . ? O1 Y2 Y1 39.3(3) 8_656 . ? O1 Y2 Y1 39.3(3) 11_466 . ? O2 P1 O3 111.3(11) . 18_356 ? O2 P1 O1 110.6(11) . . ? O3 P1 O1 111.7(8) 18_356 . ? O2 P1 O4 112.1(8) . . ? O3 P1 O4 106.6(9) 18_356 . ? O1 P1 O4 104.3(7) . . ? P1 O1 Y1 137.7(10) . . ? P1 O1 Y2 124.9(8) . . ? Y1 O1 Y2 97.3(5) . . ? P1 O2 Y2 124.1(11) . 15_546 ? P1 O3 Y1 152.4(10) 24_565 . ? P1 O4 P1 128.8(12) 15_546 . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.27 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.027 _refine_diff_density_min -1.504 _refine_diff_density_rms 0.261 _database_code_depnum_ccdc_archive 'CCDC 948280' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_hohedp _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H8 Ho2 O11.50 P3' _chemical_formula_weight 650.86 _chemical_absolute_configuration unk 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' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M I2(1)3 _symmetry_space_group_name_Hall 'I 2b 2c 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-x+1/2, y+1, -z+1' 'x+1, -y+1, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1, -x+1, -y+1/2' '-z+1, -x+1/2, y+1' '-z+1/2, x+1, -y+1' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1, -x+1' 'y+1, -z+1, -x+1/2' '-y+1, -z+1/2, x+1' _cell_length_a 13.5330(4) _cell_length_b 13.5330(4) _cell_length_c 13.5330(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2478.46(13) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 576 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 21.57 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2376 _exptl_absorpt_coefficient_mu 13.119 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5600 _exptl_absorpt_correction_T_max 0.6219 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 4801 _diffrn_reflns_av_R_equivalents 0.0834 _diffrn_reflns_av_sigmaI/netI 0.0846 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 30.43 _reflns_number_total 1251 _reflns_number_gt 986 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Due to the disorder of C1, C2 and O4 some restraints commands were used as follows: EADP O4b C2b EXYZ O4b C2b EADP O4a C2a EXYZ O4a C2a Isor 0.01 O4b C1 C2b part 1 O4A 3 0.340926 0.482972 0.876880 20.50000 0.16680 0.06606 = 0.14428 0.04729 0.12387 0.05738 C2A 1 0.340926 0.482972 0.876880 20.50000 0.16680 0.06606 = 0.14428 0.04729 0.12387 0.05738 part 2 O4B 3 0.268387 0.486257 0.792968 -20.50000 0.05275 0.05385 = 0.05723 0.00111 0.00249 -0.00340 C2B 1 0.268387 0.486257 0.792968 -20.50000 0.05275 0.05385 = 0.05723 0.00111 0.00249 -0.00340 part 0 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^)+(0.0439P)^2^+16.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(5) _refine_ls_number_reflns 1251 _refine_ls_number_parameters 71 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0730 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1148 _refine_ls_wR_factor_gt 0.1022 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.062 _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 Ho1 Ho 0.67772(5) 0.32228(5) 0.82228(5) 0.0174(2) Uani 1 3 d S . . Ho2 Ho 0.52840(5) 0.47160(5) 0.97160(5) 0.0279(3) Uani 1 3 d S . . P1 P 0.7698(3) 0.5564(3) 0.8907(3) 0.0212(7) Uani 1 1 d . . . O1 O 0.6893(7) 0.4774(8) 0.8918(7) 0.026(2) Uani 1 1 d . A . O2 O 0.4923(10) 0.5986(9) 0.8742(8) 0.041(3) Uani 1 1 d . A . O3 O 0.6214(7) 0.1974(8) 0.7372(8) 0.030(2) Uani 1 1 d . . . O4A O 0.341(3) 0.483(2) 0.877(3) 0.13(3) Uani 0.33(2) 1 d P A 1 C2A C 0.341(3) 0.483(2) 0.877(3) 0.13(3) Uani 0.33(2) 1 d P A 1 O4B O 0.268(4) 0.486(4) 0.793(4) 0.055(18) Uani 0.17(2) 1 d PU . 2 C2B C 0.268(4) 0.486(4) 0.793(4) 0.055(18) Uani 0.17(2) 1 d PU . 2 O5 O 0.4284(11) 0.5716(11) 1.0716(11) 0.079(9) Uani 0.33 1 d P A . C1 C 0.3660(15) 0.5000 0.7500 0.031(5) Uani 1 2 d SU . . 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 Ho1 0.0174(2) 0.0174(2) 0.0174(2) 0.0023(2) -0.0023(2) -0.0023(2) Ho2 0.0279(3) 0.0279(3) 0.0279(3) -0.0005(3) 0.0005(3) 0.0005(3) P1 0.0252(19) 0.0177(17) 0.0208(18) 0.0105(14) -0.0072(14) -0.0061(13) O1 0.028(5) 0.027(5) 0.021(5) -0.003(4) -0.002(4) -0.018(5) O2 0.057(8) 0.034(6) 0.033(6) 0.000(5) 0.000(6) 0.020(6) O3 0.024(5) 0.031(6) 0.036(6) -0.005(5) -0.001(5) -0.012(5) O4A 0.17(5) 0.07(2) 0.14(4) 0.05(2) 0.12(4) 0.06(2) C2A 0.17(5) 0.07(2) 0.14(4) 0.05(2) 0.12(4) 0.06(2) O4B 0.053(19) 0.054(19) 0.057(19) 0.001(7) 0.002(7) -0.003(7) C2B 0.053(19) 0.054(19) 0.057(19) 0.001(7) 0.002(7) -0.003(7) O5 0.079(9) 0.079(9) 0.079(9) -0.026(7) 0.026(7) 0.026(7) C1 0.014(7) 0.027(8) 0.052(9) 0.003(7) 0.000 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 Ho1 O3 2.182(10) . ? Ho1 O3 2.182(10) 10_646 ? Ho1 O3 2.182(10) 7_665 ? Ho1 O1 2.306(10) . ? Ho1 O1 2.306(10) 10_646 ? Ho1 O1 2.306(10) 7_665 ? Ho1 Ho2 3.5000(16) . ? Ho2 O2 2.220(12) . ? Ho2 O2 2.220(12) 7_665 ? Ho2 O2 2.220(12) 10_646 ? Ho2 O5 2.34(2) . ? Ho2 O1 2.431(10) . ? Ho2 O1 2.432(10) 7_665 ? Ho2 O1 2.432(10) 10_646 ? Ho2 O4A 2.85(6) . ? Ho2 C2A 2.85(6) 10_646 ? Ho2 O4A 2.85(6) 10_646 ? Ho2 C2A 2.85(6) 7_665 ? P1 O3 1.485(10) 20_645 ? P1 O1 1.527(10) . ? P1 O2 1.567(12) 18_456 ? P1 C1 1.834(12) 18_456 ? O2 P1 1.567(12) 24_564 ? O3 P1 1.485(10) 23_456 ? O4A C1 1.77(4) . ? O4B C2B 1.22(11) 16_456 ? O4B O4B 1.22(11) 16_456 ? O4B C1 1.45(5) . ? C1 C2B 1.45(5) 16_456 ? C1 O4B 1.45(5) 16_456 ? C1 C2A 1.77(4) 16_456 ? C1 O4A 1.77(4) 16_456 ? C1 P1 1.834(12) 24_564 ? C1 P1 1.834(12) 10_646 ? 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 Ho1 O3 92.6(4) . 10_646 ? O3 Ho1 O3 92.6(4) . 7_665 ? O3 Ho1 O3 92.6(4) 10_646 7_665 ? O3 Ho1 O1 160.7(4) . . ? O3 Ho1 O1 106.6(4) 10_646 . ? O3 Ho1 O1 87.8(4) 7_665 . ? O3 Ho1 O1 87.8(4) . 10_646 ? O3 Ho1 O1 160.7(4) 10_646 10_646 ? O3 Ho1 O1 106.6(4) 7_665 10_646 ? O1 Ho1 O1 73.6(4) . 10_646 ? O3 Ho1 O1 106.6(4) . 7_665 ? O3 Ho1 O1 87.8(4) 10_646 7_665 ? O3 Ho1 O1 160.7(4) 7_665 7_665 ? O1 Ho1 O1 73.6(4) . 7_665 ? O1 Ho1 O1 73.6(4) 10_646 7_665 ? O3 Ho1 Ho2 123.4(3) . . ? O3 Ho1 Ho2 123.4(3) 10_646 . ? O3 Ho1 Ho2 123.4(3) 7_665 . ? O1 Ho1 Ho2 43.8(2) . . ? O1 Ho1 Ho2 43.8(2) 10_646 . ? O1 Ho1 Ho2 43.8(2) 7_665 . ? O2 Ho2 O2 114.8(2) . 7_665 ? O2 Ho2 O2 114.8(2) . 10_646 ? O2 Ho2 O2 114.8(2) 7_665 10_646 ? O2 Ho2 O5 76.6(3) . . ? O2 Ho2 O5 76.6(3) 7_665 . ? O2 Ho2 O5 76.6(3) 10_646 . ? O2 Ho2 O1 84.8(4) . . ? O2 Ho2 O1 78.8(4) 7_665 . ? O2 Ho2 O1 144.1(4) 10_646 . ? O5 Ho2 O1 139.0(2) . . ? O2 Ho2 O1 144.1(4) . 7_665 ? O2 Ho2 O1 84.7(4) 7_665 7_665 ? O2 Ho2 O1 78.8(4) 10_646 7_665 ? O5 Ho2 O1 139.0(2) . 7_665 ? O1 Ho2 O1 69.2(4) . 7_665 ? O2 Ho2 O1 78.8(4) . 10_646 ? O2 Ho2 O1 144.1(4) 7_665 10_646 ? O2 Ho2 O1 84.7(4) 10_646 10_646 ? O5 Ho2 O1 139.0(2) . 10_646 ? O1 Ho2 O1 69.2(4) . 10_646 ? O1 Ho2 O1 69.2(4) 7_665 10_646 ? O2 Ho2 O4A 59.7(7) . . ? O2 Ho2 O4A 150.0(7) 7_665 . ? O2 Ho2 O4A 56.0(7) 10_646 . ? O5 Ho2 O4A 73.4(7) . . ? O1 Ho2 O4A 126.6(6) . . ? O1 Ho2 O4A 117.3(8) 7_665 . ? O1 Ho2 O4A 65.9(8) 10_646 . ? O2 Ho2 C2A 150.0(7) . 10_646 ? O2 Ho2 C2A 56.0(7) 7_665 10_646 ? O2 Ho2 C2A 59.7(7) 10_646 10_646 ? O5 Ho2 C2A 73.4(7) . 10_646 ? O1 Ho2 C2A 117.3(8) . 10_646 ? O1 Ho2 C2A 65.9(8) 7_665 10_646 ? O1 Ho2 C2A 126.6(6) 10_646 10_646 ? O4A Ho2 C2A 112.2(6) . 10_646 ? O2 Ho2 O4A 150.0(7) . 10_646 ? O2 Ho2 O4A 56.0(7) 7_665 10_646 ? O2 Ho2 O4A 59.7(7) 10_646 10_646 ? O5 Ho2 O4A 73.4(7) . 10_646 ? O1 Ho2 O4A 117.3(8) . 10_646 ? O1 Ho2 O4A 65.9(8) 7_665 10_646 ? O1 Ho2 O4A 126.6(6) 10_646 10_646 ? O4A Ho2 O4A 112.2(6) . 10_646 ? C2A Ho2 O4A 0.0(17) 10_646 10_646 ? O2 Ho2 C2A 56.0(7) . 7_665 ? O2 Ho2 C2A 59.7(7) 7_665 7_665 ? O2 Ho2 C2A 150.0(7) 10_646 7_665 ? O5 Ho2 C2A 73.4(7) . 7_665 ? O1 Ho2 C2A 65.9(8) . 7_665 ? O1 Ho2 C2A 126.6(6) 7_665 7_665 ? O1 Ho2 C2A 117.3(8) 10_646 7_665 ? O4A Ho2 C2A 112.2(6) . 7_665 ? C2A Ho2 C2A 112.2(6) 10_646 7_665 ? O4A Ho2 C2A 112.2(6) 10_646 7_665 ? O3 P1 O1 112.2(6) 20_645 . ? O3 P1 O2 112.4(6) 20_645 18_456 ? O1 P1 O2 110.3(7) . 18_456 ? O3 P1 C1 107.4(7) 20_645 18_456 ? O1 P1 C1 106.8(5) . 18_456 ? O2 P1 C1 107.3(5) 18_456 18_456 ? P1 O1 Ho1 133.0(6) . . ? P1 O1 Ho2 131.7(6) . . ? Ho1 O1 Ho2 95.2(3) . . ? P1 O2 Ho2 134.4(7) 24_564 . ? P1 O3 Ho1 149.6(7) 23_456 . ? C1 O4A Ho2 105.9(18) . . ? C2B O4B O4B 0(5) 16_456 16_456 ? C2B O4B C1 65(2) 16_456 . ? O4B O4B C1 65(2) 16_456 . ? O4B C1 C2B 50(4) . 16_456 ? O4B C1 O4B 50(4) . 16_456 ? C2B C1 O4B 0.0(17) 16_456 16_456 ? O4B C1 C2A 103(3) . 16_456 ? C2B C1 C2A 55(2) 16_456 16_456 ? O4B C1 C2A 55(2) 16_456 16_456 ? O4B C1 O4A 103(3) . 16_456 ? C2B C1 O4A 55(2) 16_456 16_456 ? O4B C1 O4A 55(2) 16_456 16_456 ? C2A C1 O4A 0(3) 16_456 16_456 ? O4B C1 O4A 55(2) . . ? C2B C1 O4A 103(3) 16_456 . ? O4B C1 O4A 103(3) 16_456 . ? C2A C1 O4A 158(4) 16_456 . ? O4A C1 O4A 158(4) 16_456 . ? O4B C1 P1 124(2) . 24_564 ? C2B C1 P1 118(2) 16_456 24_564 ? O4B C1 P1 118(2) 16_456 24_564 ? C2A C1 P1 98.4(10) 16_456 24_564 ? O4A C1 P1 98.4(10) 16_456 24_564 ? O4A C1 P1 94.2(17) . 24_564 ? O4B C1 P1 118(2) . 10_646 ? C2B C1 P1 124(2) 16_456 10_646 ? O4B C1 P1 124(2) 16_456 10_646 ? C2A C1 P1 94.2(16) 16_456 10_646 ? O4A C1 P1 94.2(16) 16_456 10_646 ? O4A C1 P1 98.4(10) . 10_646 ? P1 C1 P1 110.1(11) 24_564 10_646 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 30.43 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.689 _refine_diff_density_min -1.993 _refine_diff_density_rms 0.313 _database_code_depnum_ccdc_archive 'CCDC 948281'