# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_year 2009 _publ_contact_author_name 'Mark Weller' _publ_contact_author_email MTW@SOTON.AC.UK _publ_section_title ; Cerium (IV) Fluoride and Fluoride-Arsenate Frameworks ; loop_ _publ_author_name 'Mark Weller' 'Jessica Rouse' # Attachment 'Structure 3 CeAsO4F.cif' data_2009structure3 _database_code_depnum_ccdc_archive 'CCDC 737292' _chemical_compound_source ? _database_code_CSD 9JAA0016 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'As Ce F O4' _chemical_formula_weight 298.04 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 8.6572(4) _cell_length_b 7.0511(3) _cell_length_c 6.5731(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 401.24(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5925 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.934 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 19.441 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1122 _exptl_absorpt_correction_T_max 0.1122 _exptl_absorpt_process_details ; SADABS V2.10 (Sheldrick, G.M., 2003) ; _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 5713 reflections reduced R(int) from 0.2086 to 0.0973 Ratio of minimum to maximum apparent transmission: 0.710537 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5482 _diffrn_reflns_av_R_equivalents 0.0828 _diffrn_reflns_av_sigmaI/netI 0.0370 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.89 _diffrn_reflns_theta_max 27.52 _reflns_number_total 504 _reflns_number_gt 456 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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^ > 2\s(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^)+(0.0153P)^2^+16.4767P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 504 _refine_ls_number_parameters 32 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.0859 _refine_ls_wR_factor_gt 0.0822 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.157 _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 Ce1 Ce 0.45715(8) 0.7500 0.14482(10) 0.0068(2) Uani 1 2 d S . . As1 As 0.10387(15) 0.7500 -0.17569(19) 0.0077(3) Uani 1 2 d S . . O1 O 0.0708(7) 0.5678(9) -0.3384(9) 0.0097(9) Uani 1 1 d . . . O2 O -0.0199(10) 0.7500 0.0172(14) 0.0097(9) Uani 1 2 d S . . O3 O 0.2873(10) 0.7500 -0.1025(13) 0.0097(9) Uani 1 2 d S . . F1 F 0.7122(8) 0.7500 0.1997(11) 0.0111(16) 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 Ce1 0.0077(4) 0.0081(4) 0.0047(3) 0.000 0.0001(3) 0.000 As1 0.0097(6) 0.0083(6) 0.0051(6) 0.000 0.0001(5) 0.000 O1 0.010(2) 0.012(2) 0.007(2) 0.003(2) -0.0014(17) 0.000(3) O2 0.010(2) 0.012(2) 0.007(2) 0.003(2) -0.0014(17) 0.000(3) O3 0.010(2) 0.012(2) 0.007(2) 0.003(2) -0.0014(17) 0.000(3) F1 0.003(3) 0.020(4) 0.011(4) 0.000 0.000(3) 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 O3 2.192(9) . ? Ce1 O2 2.230(9) 6_656 ? Ce1 F1 2.238(7) . ? Ce1 O1 2.257(7) 2_565 ? Ce1 O1 2.257(7) 8_666 ? Ce1 F1 2.354(7) 6_556 ? Ce1 O1 2.584(6) 6_655 ? Ce1 O1 2.584(6) 4_564 ? Ce1 As1 3.3349(14) 6_655 ? As1 O3 1.660(9) . ? As1 O2 1.660(9) . ? As1 O1 1.696(7) . ? As1 O1 1.696(7) 7_575 ? As1 Ce1 3.3349(14) 6 ? O1 Ce1 2.257(7) 2_564 ? O1 Ce1 2.584(6) 6 ? O2 Ce1 2.230(9) 6_556 ? F1 Ce1 2.354(7) 6_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ce1 O2 143.0(3) . 6_656 ? O3 Ce1 F1 141.4(3) . . ? O2 Ce1 F1 75.6(3) 6_656 . ? O3 Ce1 O1 87.95(16) . 2_565 ? O2 Ce1 O1 87.75(16) 6_656 2_565 ? F1 Ce1 O1 95.63(16) . 2_565 ? O3 Ce1 O1 87.95(16) . 8_666 ? O2 Ce1 O1 87.75(16) 6_656 8_666 ? F1 Ce1 O1 95.63(16) . 8_666 ? O1 Ce1 O1 166.4(3) 2_565 8_666 ? O3 Ce1 F1 73.6(3) . 6_556 ? O2 Ce1 F1 69.4(3) 6_656 6_556 ? F1 Ce1 F1 144.99(6) . 6_556 ? O1 Ce1 F1 83.22(16) 2_565 6_556 ? O1 Ce1 F1 83.22(16) 8_666 6_556 ? O3 Ce1 O1 71.2(2) . 6_655 ? O2 Ce1 O1 138.0(2) 6_656 6_655 ? F1 Ce1 O1 75.5(2) . 6_655 ? O1 Ce1 O1 65.5(2) 2_565 6_655 ? O1 Ce1 O1 124.94(17) 8_666 6_655 ? F1 Ce1 O1 132.98(19) 6_556 6_655 ? O3 Ce1 O1 71.2(2) . 4_564 ? O2 Ce1 O1 138.0(2) 6_656 4_564 ? F1 Ce1 O1 75.5(2) . 4_564 ? O1 Ce1 O1 124.94(17) 2_565 4_564 ? O1 Ce1 O1 65.5(2) 8_666 4_564 ? F1 Ce1 O1 132.98(19) 6_556 4_564 ? O1 Ce1 O1 59.6(3) 6_655 4_564 ? O3 Ce1 As1 64.5(2) . 6_655 ? O2 Ce1 As1 152.5(2) 6_656 6_655 ? F1 Ce1 As1 76.88(19) . 6_655 ? O1 Ce1 As1 94.94(15) 2_565 6_655 ? O1 Ce1 As1 94.94(15) 8_666 6_655 ? F1 Ce1 As1 138.13(18) 6_556 6_655 ? O1 Ce1 As1 30.02(15) 6_655 6_655 ? O1 Ce1 As1 30.02(15) 4_564 6_655 ? O3 Ce1 Ce1 77.03(11) . 5_665 ? O2 Ce1 Ce1 116.69(6) 6_656 5_665 ? F1 Ce1 Ce1 84.01(9) . 5_665 ? O1 Ce1 Ce1 35.24(15) 2_565 5_665 ? O1 Ce1 Ce1 154.37(16) 8_666 5_665 ? F1 Ce1 Ce1 111.52(7) 6_556 5_665 ? O1 Ce1 Ce1 30.26(15) 6_655 5_665 ? O1 Ce1 Ce1 89.80(15) 4_564 5_665 ? As1 Ce1 Ce1 59.912(17) 6_655 5_665 ? O3 Ce1 Ce1 77.03(11) . 5_675 ? O2 Ce1 Ce1 116.69(6) 6_656 5_675 ? F1 Ce1 Ce1 84.01(9) . 5_675 ? O1 Ce1 Ce1 154.37(16) 2_565 5_675 ? O1 Ce1 Ce1 35.24(15) 8_666 5_675 ? F1 Ce1 Ce1 111.52(7) 6_556 5_675 ? O1 Ce1 Ce1 89.80(15) 6_655 5_675 ? O1 Ce1 Ce1 30.26(15) 4_564 5_675 ? As1 Ce1 Ce1 59.912(17) 6_655 5_675 ? Ce1 Ce1 Ce1 119.81(3) 5_665 5_675 ? O3 As1 O2 113.3(4) . . ? O3 As1 O1 110.1(3) . . ? O2 As1 O1 111.9(3) . . ? O3 As1 O1 110.1(3) . 7_575 ? O2 As1 O1 111.9(3) . 7_575 ? O1 As1 O1 98.5(4) . 7_575 ? O3 As1 Ce1 129.2(3) . 6 ? O2 As1 Ce1 117.4(3) . 6 ? O1 As1 Ce1 49.7(2) . 6 ? O1 As1 Ce1 49.7(2) 7_575 6 ? As1 O1 Ce1 143.3(3) . 2_564 ? As1 O1 Ce1 100.3(3) . 6 ? Ce1 O1 Ce1 114.5(2) 2_564 6 ? As1 O2 Ce1 144.9(5) . 6_556 ? As1 O3 Ce1 149.0(5) . . ? Ce1 F1 Ce1 163.5(4) . 6_656 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.614 _refine_diff_density_min -1.890 _refine_diff_density_rms 0.402 # Attachment 'Structure 2 Ce4(AsO4)6(H2O)F3.cif' data_structure2 _database_code_depnum_ccdc_archive 'CCDC 737293' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H26 As6 Ce4 F3 N5 O27' _chemical_formula_weight 1595.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3894(3) _cell_length_b 9.5285(3) _cell_length_c 18.4963(5) _cell_angle_alpha 91.234(2) _cell_angle_beta 104.024(2) _cell_angle_gamma 114.293(2) _cell_volume 1449.51(8) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 143424 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 33.14 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.655 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1468 _exptl_absorpt_coefficient_mu 13.089 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0587 _exptl_absorpt_correction_T_max 0.3544 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30092 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5106 _reflns_number_gt 4661 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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^ > 2\s(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. An isotropic thermal restraint was used to reduce the oblate nature of the oxygen temperature factors for O22 and O52. The hydrogen atoms shave been included in the formula, but not the refinement. ; _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^)+(0.0307P)^2^+9.7864P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5106 _refine_ls_number_parameters 406 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0330 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0851 _refine_ls_wR_factor_gt 0.0829 _refine_ls_goodness_of_fit_ref 1.192 _refine_ls_restrained_S_all 1.191 _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 As1 As 0.67602(8) 0.87576(7) 0.38105(3) 0.00608(15) Uani 1 1 d . . . As2 As 0.04087(8) 0.97357(7) 0.12979(3) 0.00586(15) Uani 1 1 d . . . As3 As -0.10710(8) 0.51862(7) 0.13040(3) 0.00599(15) Uani 1 1 d . . . As4 As 0.12901(8) 1.00616(7) 0.37343(3) 0.00594(15) Uani 1 1 d . . . As5 As -0.00969(8) 0.54618(7) 0.36777(3) 0.00576(15) Uani 1 1 d . . . As6 As 0.34032(8) 0.64637(7) 0.11259(3) 0.00515(15) Uani 1 1 d . . . Ce1 Ce 0.26309(4) 0.82953(4) 0.275444(19) 0.00556(11) Uani 1 1 d . . . Ce2 Ce -0.03654(4) 0.28594(4) 0.033012(19) 0.00527(11) Uani 1 1 d . . . Ce3 Ce 0.04370(4) 1.22606(4) 0.473955(19) 0.00561(11) Uani 1 1 d . . . Ce4 Ce -0.24543(4) 0.69527(4) 0.222506(19) 0.00533(11) Uani 1 1 d . . . N1 N -0.1954(7) 1.1504(7) 0.2486(3) 0.0141(12) Uani 1 1 d . . . N2 N 0.6079(7) 0.2154(7) 0.4943(3) 0.0178(13) Uani 1 1 d . . . N3 N 0.2292(8) 0.3768(9) 0.2545(4) 0.0304(17) Uani 1 1 d . . . N4 N 0.4600(8) 0.4621(9) 0.4071(3) 0.037(2) Uani 1 1 d . . . N5 N 0.5624(9) 0.2970(8) 0.3310(4) 0.0344(18) Uani 1 1 d . . . O11 O 0.4743(5) 0.8174(5) 0.3660(2) 0.0087(9) Uani 1 1 d . . . O12 O 0.7765(5) 1.0682(5) 0.4129(2) 0.0090(9) Uani 1 1 d . . . O13 O 0.7183(6) 0.8455(6) 0.2998(2) 0.0129(10) Uani 1 1 d . . . O14 O 0.7255(6) 0.7645(5) 0.4434(2) 0.0113(10) Uani 1 1 d . . . O21 O -0.1352(5) 0.8991(5) 0.1546(2) 0.0100(10) Uani 1 1 d . . . O22 O 0.0696(5) 1.1544(5) 0.1107(2) 0.0078(9) Uani 1 1 d U . . O23 O 0.2064(5) 0.9925(5) 0.1968(2) 0.0093(9) Uani 1 1 d . . . O24 O 0.0167(6) 0.8628(5) 0.0508(3) 0.0135(10) Uani 1 1 d . . . O31 O -0.0030(5) 0.6762(5) 0.1956(2) 0.0081(9) Uani 1 1 d . . . O32 O -0.2954(5) 0.5059(5) 0.1196(2) 0.0106(10) Uani 1 1 d . . . O33 O -0.0883(6) 0.3537(5) 0.1483(2) 0.0099(10) Uani 1 1 d . . . O34 O -0.0410(6) 0.5409(5) 0.0524(2) 0.0098(10) Uani 1 1 d . . . O41 O 0.0257(5) 0.8625(5) 0.3008(2) 0.0098(10) Uani 1 1 d . . . O42 O 0.3162(5) 1.0125(5) 0.3848(3) 0.0111(10) Uani 1 1 d . . . O43 O 0.1230(6) 1.1793(5) 0.3622(2) 0.0102(10) Uani 1 1 d . . . O44 O 0.0503(6) 0.9703(5) 0.4474(2) 0.0091(9) Uani 1 1 d . . . O51 O -0.1743(6) 0.5444(6) 0.3042(3) 0.0127(10) Uani 1 1 d . . . O52 O 0.0316(6) 0.6623(5) 0.4477(2) 0.0113(10) Uani 1 1 d U . . O53 O -0.0596(6) 0.3599(5) 0.3834(2) 0.0098(9) Uani 1 1 d . . . O54 O 0.1559(5) 0.6172(5) 0.3348(2) 0.0106(10) Uani 1 1 d . . . O61 O 0.3019(6) 0.6905(5) 0.1924(2) 0.0098(10) Uani 1 1 d . . . O62 O 0.2810(5) 0.7447(5) 0.0448(2) 0.0086(9) Uani 1 1 d . . . O63 O 0.5407(5) 0.7026(5) 0.1253(2) 0.0069(9) Uani 1 1 d . . . O64 O 0.2330(5) 0.4514(5) 0.0861(2) 0.0079(9) Uani 1 1 d . . . O1 O -0.2730(5) 0.0519(5) 0.0576(2) 0.0112(10) Uani 1 1 d . . . OW1 O 0.4637(6) 0.0581(5) 0.1049(3) 0.0146(10) Uani 1 1 d . . . OW2 O 0.4077(7) 0.2982(7) 0.0292(3) 0.0299(13) Uani 1 1 d . . . F1 F -0.4696(5) 0.5136(6) 0.2367(2) 0.0245(10) Uani 1 1 d . . . F2 F 0.4925(5) 1.0165(5) 0.2596(2) 0.0174(9) Uani 1 1 d . . . F3 F 0.2421(5) 1.4588(5) 0.4827(2) 0.0216(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.0063(3) 0.0072(3) 0.0051(3) -0.0003(2) 0.0013(2) 0.0034(3) As2 0.0081(3) 0.0060(3) 0.0054(3) 0.0017(2) 0.0030(3) 0.0043(3) As3 0.0077(3) 0.0056(3) 0.0057(3) 0.0004(2) 0.0028(2) 0.0033(3) As4 0.0071(3) 0.0062(3) 0.0050(3) 0.0002(2) 0.0026(3) 0.0028(3) As5 0.0074(3) 0.0058(3) 0.0048(3) 0.0009(2) 0.0021(2) 0.0032(3) As6 0.0052(3) 0.0062(3) 0.0047(3) 0.0004(2) 0.0016(2) 0.0030(3) Ce1 0.0060(2) 0.00652(19) 0.00474(18) 0.00052(14) 0.00194(14) 0.00304(15) Ce2 0.0068(2) 0.00501(19) 0.00491(19) 0.00059(14) 0.00226(14) 0.00311(15) Ce3 0.0071(2) 0.00560(19) 0.00481(19) 0.00053(14) 0.00197(14) 0.00318(15) Ce4 0.0061(2) 0.00570(19) 0.00489(18) 0.00036(14) 0.00187(14) 0.00298(15) N1 0.017(3) 0.012(3) 0.010(3) 0.003(2) 0.002(2) 0.005(3) N2 0.010(3) 0.018(3) 0.018(3) 0.004(3) -0.003(2) 0.002(3) N3 0.015(4) 0.039(4) 0.034(4) 0.025(3) 0.005(3) 0.009(3) N4 0.022(4) 0.049(5) 0.010(3) -0.001(3) 0.007(3) -0.014(3) N5 0.034(4) 0.016(4) 0.028(4) 0.014(3) -0.004(3) -0.007(3) O11 0.005(2) 0.013(2) 0.008(2) 0.0035(18) 0.0016(18) 0.0046(19) O12 0.011(2) 0.010(2) 0.006(2) 0.0021(18) 0.0011(18) 0.005(2) O13 0.014(3) 0.019(3) 0.010(2) -0.0020(19) 0.0052(19) 0.010(2) O14 0.009(2) 0.012(2) 0.012(2) 0.0036(19) -0.0004(19) 0.005(2) O21 0.007(2) 0.012(2) 0.015(2) 0.0017(19) 0.0056(19) 0.005(2) O22 0.011(2) 0.004(2) 0.008(2) 0.0040(16) 0.0023(17) 0.0031(17) O23 0.007(2) 0.009(2) 0.013(2) 0.0066(18) 0.0022(18) 0.0043(19) O24 0.021(3) 0.011(2) 0.012(2) -0.0006(19) 0.006(2) 0.009(2) O31 0.006(2) 0.009(2) 0.008(2) -0.0022(18) 0.0003(18) 0.0040(19) O32 0.008(2) 0.011(2) 0.012(2) -0.0031(19) 0.0026(19) 0.0034(19) O33 0.013(2) 0.010(2) 0.011(2) 0.0012(18) 0.0061(19) 0.007(2) O34 0.016(3) 0.011(2) 0.006(2) 0.0013(18) 0.0062(19) 0.007(2) O41 0.011(2) 0.009(2) 0.007(2) -0.0047(18) 0.0006(18) 0.004(2) O42 0.007(2) 0.011(2) 0.014(2) -0.0024(19) 0.0020(19) 0.004(2) O43 0.011(2) 0.010(2) 0.012(2) 0.0054(18) 0.0076(19) 0.005(2) O44 0.014(2) 0.010(2) 0.006(2) 0.0003(18) 0.0059(19) 0.006(2) O51 0.011(3) 0.018(3) 0.011(2) 0.0079(19) 0.0042(19) 0.008(2) O52 0.018(2) 0.008(2) 0.010(2) -0.0024(17) 0.0052(18) 0.0063(18) O53 0.015(2) 0.005(2) 0.010(2) 0.0045(18) 0.0056(19) 0.003(2) O54 0.009(2) 0.013(2) 0.010(2) 0.0013(19) 0.0048(19) 0.004(2) O61 0.012(2) 0.015(2) 0.007(2) 0.0022(18) 0.0048(18) 0.009(2) O62 0.009(2) 0.004(2) 0.013(2) 0.0038(18) 0.0029(18) 0.0035(19) O63 0.005(2) 0.009(2) 0.007(2) 0.0028(17) 0.0024(17) 0.0023(19) O64 0.011(2) 0.006(2) 0.007(2) 0.0003(17) 0.0014(18) 0.0047(19) O1 0.010(2) 0.010(2) 0.012(2) 0.0032(18) 0.0024(19) 0.0030(19) OW1 0.017(3) 0.012(2) 0.017(2) 0.0026(19) 0.007(2) 0.006(2) OW2 0.022(3) 0.028(3) 0.035(3) 0.001(3) 0.004(3) 0.008(3) F1 0.016(2) 0.038(3) 0.025(2) 0.021(2) 0.0092(19) 0.015(2) F2 0.008(2) 0.020(2) 0.017(2) 0.0099(17) 0.0007(16) 0.0013(17) F3 0.016(2) 0.011(2) 0.031(2) 0.0099(18) 0.0028(19) 0.0016(18) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 As1 O11 1.687(4) . ? As1 O12 1.691(4) . ? As1 O13 1.693(4) . ? As1 O14 1.694(4) . ? As2 O23 1.677(4) . ? As2 O22 1.690(4) . ? As2 O21 1.692(4) . ? As2 O24 1.696(4) . ? As3 O31 1.675(4) . ? As3 O33 1.683(4) . ? As3 O32 1.683(4) . ? As3 O34 1.689(4) . ? As3 Ce4 3.1891(7) . ? As3 Ce2 3.1960(7) . ? As4 O41 1.678(4) . ? As4 O44 1.684(4) . ? As4 O43 1.689(4) . ? As4 O42 1.694(4) . ? As4 Ce1 3.2279(7) . ? As4 Ce3 3.2287(7) . ? As5 O53 1.690(4) . ? As5 O54 1.691(5) . ? As5 O52 1.691(4) . ? As5 O51 1.693(5) . ? As6 O63 1.683(4) . ? As6 O61 1.687(4) . ? As6 O64 1.700(4) . ? As6 O62 1.704(4) . ? Ce1 O61 2.197(4) . ? Ce1 F2 2.252(4) . ? Ce1 O23 2.283(4) . ? Ce1 O54 2.295(5) . ? Ce1 O11 2.311(4) . ? Ce1 O31 2.382(4) . ? Ce1 O42 2.454(4) . ? Ce1 O41 2.522(4) . ? Ce2 O24 2.170(4) 2_565 ? Ce2 O22 2.245(4) 1_545 ? Ce2 O62 2.292(4) 2_565 ? Ce2 O64 2.302(4) . ? Ce2 O34 2.329(4) 2_565 ? Ce2 O33 2.430(4) . ? Ce2 O34 2.467(4) . ? Ce2 O1 2.562(5) . ? Ce3 O52 2.186(4) 2_576 ? Ce3 F3 2.203(4) . ? Ce3 O14 2.295(5) 2_676 ? Ce3 O12 2.298(5) 1_455 ? Ce3 O53 2.386(4) 1_565 ? Ce3 O44 2.404(4) 2_576 ? Ce3 O43 2.450(4) . ? Ce3 O44 2.504(4) . ? Ce4 O13 2.181(4) 1_455 ? Ce4 F1 2.188(4) . ? Ce4 O51 2.278(5) . ? Ce4 O21 2.346(5) . ? Ce4 O63 2.376(4) 1_455 ? Ce4 O32 2.413(4) . ? Ce4 O41 2.428(4) . ? Ce4 O31 2.519(4) . ? O12 Ce3 2.298(4) 1_655 ? O13 Ce4 2.181(4) 1_655 ? O14 Ce3 2.295(4) 2_676 ? O22 Ce2 2.245(4) 1_565 ? O24 Ce2 2.170(4) 2_565 ? O34 Ce2 2.329(4) 2_565 ? O44 Ce3 2.404(4) 2_576 ? O52 Ce3 2.186(4) 2_576 ? O53 Ce3 2.386(4) 1_545 ? O62 Ce2 2.292(4) 2_565 ? O63 Ce4 2.376(4) 1_655 ? 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 O11 As1 O12 109.9(2) . . ? O11 As1 O13 110.3(2) . . ? O12 As1 O13 107.8(2) . . ? O11 As1 O14 105.5(2) . . ? O12 As1 O14 113.2(2) . . ? O13 As1 O14 110.1(2) . . ? O23 As2 O22 106.9(2) . . ? O23 As2 O21 115.3(2) . . ? O22 As2 O21 105.7(2) . . ? O23 As2 O24 110.9(2) . . ? O22 As2 O24 109.6(2) . . ? O21 As2 O24 108.3(2) . . ? O31 As3 O33 119.0(2) . . ? O31 As3 O32 98.9(2) . . ? O33 As3 O32 114.5(2) . . ? O31 As3 O34 112.5(2) . . ? O33 As3 O34 97.2(2) . . ? O32 As3 O34 115.9(2) . . ? O31 As3 Ce4 51.64(15) . . ? O33 As3 Ce4 126.52(15) . . ? O32 As3 Ce4 48.01(15) . . ? O34 As3 Ce4 136.23(15) . . ? O31 As3 Ce2 138.71(15) . . ? O33 As3 Ce2 48.40(14) . . ? O32 As3 Ce2 122.33(15) . . ? O34 As3 Ce2 49.71(15) . . ? Ce4 As3 Ce2 168.81(3) . . ? O41 As4 O44 112.8(2) . . ? O41 As4 O43 117.8(2) . . ? O44 As4 O43 97.7(2) . . ? O41 As4 O42 98.6(2) . . ? O44 As4 O42 117.4(2) . . ? O43 As4 O42 113.7(2) . . ? O41 As4 Ce1 50.62(15) . . ? O44 As4 Ce1 135.48(15) . . ? O43 As4 Ce1 126.86(15) . . ? O42 As4 Ce1 48.34(15) . . ? O41 As4 Ce3 136.23(16) . . ? O44 As4 Ce3 50.00(15) . . ? O43 As4 Ce3 48.16(15) . . ? O42 As4 Ce3 125.17(15) . . ? Ce1 As4 Ce3 171.76(2) . . ? O53 As5 O54 111.5(2) . . ? O53 As5 O52 111.1(2) . . ? O54 As5 O52 107.8(2) . . ? O53 As5 O51 106.0(2) . . ? O54 As5 O51 111.0(2) . . ? O52 As5 O51 109.5(2) . . ? O63 As6 O61 111.2(2) . . ? O63 As6 O64 111.6(2) . . ? O61 As6 O64 107.5(2) . . ? O63 As6 O62 106.8(2) . . ? O61 As6 O62 109.3(2) . . ? O64 As6 O62 110.5(2) . . ? O61 Ce1 F2 82.35(16) . . ? O61 Ce1 O23 96.91(16) . . ? F2 Ce1 O23 68.95(15) . . ? O61 Ce1 O54 91.41(16) . . ? F2 Ce1 O54 145.57(15) . . ? O23 Ce1 O54 145.46(16) . . ? O61 Ce1 O11 89.61(16) . . ? F2 Ce1 O11 74.11(15) . . ? O23 Ce1 O11 141.14(16) . . ? O54 Ce1 O11 72.02(16) . . ? O61 Ce1 O31 76.06(16) . . ? F2 Ce1 O31 134.87(14) . . ? O23 Ce1 O31 74.88(16) . . ? O54 Ce1 O31 74.75(16) . . ? O11 Ce1 O31 143.34(16) . . ? O61 Ce1 O42 161.11(16) . . ? F2 Ce1 O42 83.87(15) . . ? O23 Ce1 O42 90.10(16) . . ? O54 Ce1 O42 92.69(15) . . ? O11 Ce1 O42 74.19(15) . . ? O31 Ce1 O42 122.79(14) . . ? O61 Ce1 O41 137.06(16) . . ? F2 Ce1 O41 127.30(15) . . ? O23 Ce1 O41 72.24(15) . . ? O54 Ce1 O41 78.88(15) . . ? O11 Ce1 O41 125.25(14) . . ? O31 Ce1 O41 61.01(14) . . ? O42 Ce1 O41 61.82(14) . . ? O61 Ce1 As4 167.77(12) . . ? F2 Ce1 As4 105.22(11) . . ? O23 Ce1 As4 77.42(11) . . ? O54 Ce1 As4 87.54(11) . . ? O11 Ce1 As4 101.62(11) . . ? O31 Ce1 As4 91.93(10) . . ? O42 Ce1 As4 31.05(11) . . ? O41 Ce1 As4 30.95(10) . . ? O24 Ce2 O22 81.45(17) 2_565 1_545 ? O24 Ce2 O62 89.44(17) 2_565 2_565 ? O22 Ce2 O62 139.91(16) 1_545 2_565 ? O24 Ce2 O64 100.85(17) 2_565 . ? O22 Ce2 O64 73.40(15) 1_545 . ? O62 Ce2 O64 146.61(15) 2_565 . ? O24 Ce2 O34 79.80(16) 2_565 2_565 ? O22 Ce2 O34 137.85(16) 1_545 2_565 ? O62 Ce2 O34 77.22(16) 2_565 2_565 ? O64 Ce2 O34 73.58(16) . 2_565 ? O24 Ce2 O33 156.55(16) 2_565 . ? O22 Ce2 O33 80.02(15) 1_545 . ? O62 Ce2 O33 95.56(15) 2_565 . ? O64 Ce2 O33 87.48(15) . . ? O34 Ce2 O33 123.65(15) 2_565 . ? O24 Ce2 O34 140.93(16) 2_565 . ? O22 Ce2 O34 132.31(15) 1_545 . ? O62 Ce2 O34 75.42(15) 2_565 . ? O64 Ce2 O34 76.78(15) . . ? O34 Ce2 O34 61.93(17) 2_565 . ? O33 Ce2 O34 62.19(14) . . ? O24 Ce2 O1 89.97(16) 2_565 . ? O22 Ce2 O1 72.31(15) 1_545 . ? O62 Ce2 O1 68.71(15) 2_565 . ? O64 Ce2 O1 141.92(15) . . ? O34 Ce2 O1 144.50(15) 2_565 . ? O33 Ce2 O1 70.77(14) . . ? O34 Ce2 O1 116.19(14) . . ? O24 Ce2 As3 169.34(13) 2_565 . ? O22 Ce2 As3 108.93(11) 1_545 . ? O62 Ce2 As3 80.99(11) 2_565 . ? O64 Ce2 As3 84.91(10) . . ? O34 Ce2 As3 93.41(10) 2_565 . ? O33 Ce2 As3 31.19(11) . . ? O34 Ce2 As3 31.49(10) . . ? O1 Ce2 As3 90.91(10) . . ? O24 Ce2 Ce2 111.43(13) 2_565 2_565 ? O22 Ce2 Ce2 145.44(11) 1_545 2_565 ? O62 Ce2 Ce2 73.96(11) 2_565 2_565 ? O64 Ce2 Ce2 72.71(11) . 2_565 ? O34 Ce2 Ce2 31.95(10) 2_565 2_565 ? O33 Ce2 Ce2 91.95(11) . 2_565 ? O34 Ce2 Ce2 29.98(10) . 2_565 ? O1 Ce2 Ce2 136.53(10) . 2_565 ? As3 Ce2 Ce2 61.464(14) . 2_565 ? O52 Ce3 F3 85.17(17) 2_576 . ? O52 Ce3 O14 97.81(17) 2_576 2_676 ? F3 Ce3 O14 71.69(16) . 2_676 ? O52 Ce3 O12 90.49(17) 2_576 1_455 ? F3 Ce3 O12 143.74(15) . 1_455 ? O14 Ce3 O12 144.43(16) 2_676 1_455 ? O52 Ce3 O53 84.88(16) 2_576 1_565 ? F3 Ce3 O53 73.10(15) . 1_565 ? O14 Ce3 O53 144.30(17) 2_676 1_565 ? O12 Ce3 O53 70.66(15) 1_455 1_565 ? O52 Ce3 O44 77.17(16) 2_576 2_576 ? F3 Ce3 O44 139.13(15) . 2_576 ? O14 Ce3 O44 74.59(16) 2_676 2_576 ? O12 Ce3 O44 73.69(16) 1_455 2_576 ? O53 Ce3 O44 139.70(16) 1_565 2_576 ? O52 Ce3 O43 159.11(16) 2_576 . ? F3 Ce3 O43 82.20(16) . . ? O14 Ce3 O43 93.94(16) 2_676 . ? O12 Ce3 O43 89.92(15) 1_455 . ? O53 Ce3 O43 75.56(15) 1_565 . ? O44 Ce3 O43 122.82(14) 2_576 . ? O52 Ce3 O44 138.56(16) 2_576 . ? F3 Ce3 O44 126.80(16) . . ? O14 Ce3 O44 73.31(15) 2_676 . ? O12 Ce3 O44 77.63(15) 1_455 . ? O53 Ce3 O44 126.02(14) 1_565 . ? O44 Ce3 O44 61.40(16) 2_576 . ? O43 Ce3 O44 61.65(14) . . ? O52 Ce3 As4 169.54(12) 2_576 . ? F3 Ce3 As4 103.61(12) . . ? O14 Ce3 As4 79.91(11) 2_676 . ? O12 Ce3 As4 85.72(11) 1_455 . ? O53 Ce3 As4 102.97(10) 1_565 . ? O44 Ce3 As4 92.40(10) 2_576 . ? O43 Ce3 As4 30.90(10) . . ? O44 Ce3 As4 31.01(10) . . ? O13 Ce4 F1 85.11(18) 1_455 . ? O13 Ce4 O51 99.61(17) 1_455 . ? F1 Ce4 O51 72.46(16) . . ? O13 Ce4 O21 92.09(16) 1_455 . ? F1 Ce4 O21 145.23(15) . . ? O51 Ce4 O21 141.78(16) . . ? O13 Ce4 O63 89.92(16) 1_455 1_455 ? F1 Ce4 O63 74.29(15) . 1_455 ? O51 Ce4 O63 144.37(16) . 1_455 ? O21 Ce4 O63 71.05(15) . 1_455 ? O13 Ce4 O32 161.85(17) 1_455 . ? F1 Ce4 O32 82.24(17) . . ? O51 Ce4 O32 88.94(16) . . ? O21 Ce4 O32 90.93(15) . . ? O63 Ce4 O32 74.17(15) 1_455 . ? O13 Ce4 O41 75.21(16) 1_455 . ? F1 Ce4 O41 137.62(15) . . ? O51 Ce4 O41 74.35(16) . . ? O21 Ce4 O41 73.76(16) . . ? O63 Ce4 O41 141.10(15) 1_455 . ? O32 Ce4 O41 122.74(15) . . ? O13 Ce4 O31 135.52(16) 1_455 . ? F1 Ce4 O31 130.25(16) . . ? O51 Ce4 O31 73.17(15) . . ? O21 Ce4 O31 73.08(15) . . ? O63 Ce4 O31 121.88(14) 1_455 . ? O32 Ce4 O31 62.28(14) . . ? O41 Ce4 O31 60.47(14) . . ? O13 Ce4 As3 166.87(13) 1_455 . ? F1 Ce4 As3 105.01(12) . . ? O51 Ce4 As3 76.10(11) . . ? O21 Ce4 As3 84.31(10) . . ? O63 Ce4 As3 100.78(10) 1_455 . ? O32 Ce4 As3 31.23(11) . . ? O41 Ce4 As3 91.66(10) . . ? O31 Ce4 As3 31.44(10) . . ? As1 O11 Ce1 137.5(2) . . ? As1 O12 Ce3 132.7(2) . 1_655 ? As1 O13 Ce4 149.4(3) . 1_655 ? As1 O14 Ce3 137.3(3) . 2_676 ? As2 O21 Ce4 132.8(2) . . ? As2 O22 Ce2 143.2(2) . 1_565 ? As2 O23 Ce1 133.4(2) . . ? As2 O24 Ce2 165.8(3) . 2_565 ? As3 O31 Ce1 141.4(2) . . ? As3 O31 Ce4 96.92(19) . . ? Ce1 O31 Ce4 120.14(16) . . ? As3 O32 Ce4 100.8(2) . . ? As3 O33 Ce2 100.4(2) . . ? As3 O34 Ce2 143.1(2) . 2_565 ? As3 O34 Ce2 98.8(2) . . ? Ce2 O34 Ce2 118.07(17) 2_565 . ? As4 O41 Ce4 143.3(2) . . ? As4 O41 Ce1 98.4(2) . . ? Ce4 O41 Ce1 118.23(16) . . ? As4 O42 Ce1 100.6(2) . . ? As4 O43 Ce3 100.9(2) . . ? As4 O44 Ce3 142.4(2) . 2_576 ? As4 O44 Ce3 99.0(2) . . ? Ce3 O44 Ce3 118.60(16) 2_576 . ? As5 O51 Ce4 140.4(3) . . ? As5 O52 Ce3 151.4(3) . 2_576 ? As5 O53 Ce3 137.0(2) . 1_545 ? As5 O54 Ce1 132.7(2) . . ? As6 O61 Ce1 157.5(3) . . ? As6 O62 Ce2 134.9(2) . 2_565 ? As6 O63 Ce4 134.8(2) . 1_655 ? As6 O64 Ce2 135.2(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.537 _refine_diff_density_min -1.846 _refine_diff_density_rms 0.563 # Attachment 'Structure 4 CeAsO4F(H2O).cif' data_structure4 _database_code_depnum_ccdc_archive 'CCDC 737294' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H2 As Ce F O5' _chemical_formula_weight 316.06 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 5.0896(3) _cell_length_b 7.5118(5) _cell_length_c 11.8183(8) _cell_angle_alpha 90.00 _cell_angle_beta 97.740(4) _cell_angle_gamma 90.00 _cell_volume 447.72(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 10067 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.689 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 568 _exptl_absorpt_coefficient_mu 17.453 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4757 _exptl_absorpt_correction_T_max 0.7216 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4520 _diffrn_reflns_av_R_equivalents 0.1076 _diffrn_reflns_av_sigmaI/netI 0.0682 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 25.02 _reflns_number_total 785 _reflns_number_gt 645 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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^ > 2\s(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. The hydrogen atoms have been included in the formula, but not the refinement. ; _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^)+(0.0000P)^2^+68.6224P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 785 _refine_ls_number_parameters 43 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0908 _refine_ls_R_factor_gt 0.0706 _refine_ls_wR_factor_ref 0.1566 _refine_ls_wR_factor_gt 0.1467 _refine_ls_goodness_of_fit_ref 1.210 _refine_ls_restrained_S_all 1.210 _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 Ce1 Ce 0.2165(3) 0.70567(19) 0.18888(11) 0.0082(4) Uani 1 1 d . . . As1 As 0.7900(5) 0.8621(3) 0.3868(2) 0.0086(6) Uani 1 1 d . . . F1 F 0.133(2) 0.5038(17) 0.3230(11) 0.0092(14) Uani 1 1 d . . . O1 O -0.123(3) 0.888(2) 0.0779(13) 0.0092(14) Uani 1 1 d . . . O2 O 0.612(3) 0.710(2) 0.3067(13) 0.0092(14) Uani 1 1 d . . . O3 O 0.617(3) 1.049(2) 0.3940(13) 0.0092(14) Uani 1 1 d . . . O4 O 0.877(3) 0.782(2) 0.5211(13) 0.0092(14) Uani 1 1 d . . . O5 O 1.069(3) 0.901(2) 0.3272(13) 0.0092(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce1 0.0091(7) 0.0068(7) 0.0089(7) 0.0001(5) 0.0021(5) -0.0001(5) As1 0.0097(12) 0.0067(12) 0.0093(12) -0.0006(9) 0.0010(9) 0.0012(9) F1 0.011(3) 0.007(3) 0.010(3) 0.003(3) 0.000(3) 0.003(3) O1 0.011(3) 0.007(3) 0.010(3) 0.003(3) 0.000(3) 0.003(3) O2 0.011(3) 0.007(3) 0.010(3) 0.003(3) 0.000(3) 0.003(3) O3 0.011(3) 0.007(3) 0.010(3) 0.003(3) 0.000(3) 0.003(3) O4 0.011(3) 0.007(3) 0.010(3) 0.003(3) 0.000(3) 0.003(3) O5 0.011(3) 0.007(3) 0.010(3) 0.003(3) 0.000(3) 0.003(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 O3 2.186(16) 2_545 ? Ce1 O4 2.246(15) 4_575 ? Ce1 F1 2.275(13) . ? Ce1 O2 2.290(15) . ? Ce1 F1 2.376(13) 2 ? Ce1 O5 2.389(16) 1_455 ? Ce1 O1 2.445(15) . ? Ce1 O5 2.555(16) 2_645 ? As1 O3 1.664(16) . ? As1 O2 1.671(16) . ? As1 O5 1.695(16) . ? As1 O4 1.700(15) . ? F1 Ce1 2.376(13) 2_545 ? O3 Ce1 2.186(15) 2 ? O4 Ce1 2.246(15) 4_676 ? O5 Ce1 2.389(16) 1_655 ? O5 Ce1 2.555(16) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ce1 O4 88.8(6) 2_545 4_575 ? O3 Ce1 F1 75.3(5) 2_545 . ? O4 Ce1 F1 140.2(5) 4_575 . ? O3 Ce1 O2 147.8(6) 2_545 . ? O4 Ce1 O2 98.2(5) 4_575 . ? F1 Ce1 O2 79.4(5) . . ? O3 Ce1 F1 135.9(5) 2_545 2 ? O4 Ce1 F1 75.5(5) 4_575 2 ? F1 Ce1 F1 139.6(3) . 2 ? O2 Ce1 F1 76.1(5) . 2 ? O3 Ce1 O5 110.0(6) 2_545 1_455 ? O4 Ce1 O5 139.7(6) 4_575 1_455 ? F1 Ce1 O5 80.0(5) . 1_455 ? O2 Ce1 O5 84.7(5) . 1_455 ? F1 Ce1 O5 66.1(5) 2 1_455 ? O3 Ce1 O1 67.2(6) 2_545 . ? O4 Ce1 O1 79.5(5) 4_575 . ? F1 Ce1 O1 124.2(5) . . ? O2 Ce1 O1 145.0(6) . . ? F1 Ce1 O1 69.5(5) 2 . ? O5 Ce1 O1 76.1(5) 1_455 . ? O3 Ce1 O5 78.2(6) 2_545 2_645 ? O4 Ce1 O5 76.3(5) 4_575 2_645 ? F1 Ce1 O5 64.9(5) . 2_645 ? O2 Ce1 O5 73.0(5) . 2_645 ? F1 Ce1 O5 134.2(5) 2 2_645 ? O5 Ce1 O5 141.0(3) 1_455 2_645 ? O1 Ce1 O5 137.8(5) . 2_645 ? O3 Ce1 Ce1 133.5(4) 2_545 2 ? O4 Ce1 Ce1 104.7(4) 4_575 2 ? F1 Ce1 Ce1 112.8(3) . 2 ? O2 Ce1 Ce1 75.2(4) . 2 ? F1 Ce1 Ce1 29.4(3) 2 2 ? O5 Ce1 Ce1 36.9(4) 1_455 2 ? O1 Ce1 Ce1 71.9(4) . 2 ? O5 Ce1 Ce1 147.9(3) 2_645 2 ? O3 Ce1 Ce1 71.4(4) 2_545 2_545 ? O4 Ce1 Ce1 109.5(4) 4_575 2_545 ? F1 Ce1 Ce1 30.9(3) . 2_545 ? O2 Ce1 Ce1 76.7(4) . 2_545 ? F1 Ce1 Ce1 152.7(3) 2 2_545 ? O5 Ce1 Ce1 110.3(4) 1_455 2_545 ? O1 Ce1 Ce1 137.3(4) . 2_545 ? O5 Ce1 Ce1 34.2(4) 2_645 2_545 ? Ce1 Ce1 Ce1 138.07(7) 2 2_545 ? O3 As1 O2 110.8(8) . . ? O3 As1 O5 111.0(8) . . ? O2 As1 O5 107.5(7) . . ? O3 As1 O4 109.0(8) . . ? O2 As1 O4 109.7(8) . . ? O5 As1 O4 108.8(7) . . ? Ce1 F1 Ce1 119.7(5) . 2_545 ? As1 O2 Ce1 135.9(9) . . ? As1 O3 Ce1 144.7(9) . 2 ? As1 O4 Ce1 136.8(8) . 4_676 ? As1 O5 Ce1 122.5(8) . 1_655 ? As1 O5 Ce1 125.1(8) . 2_655 ? Ce1 O5 Ce1 108.8(6) 1_655 2_655 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.391 _refine_diff_density_min -2.293 _refine_diff_density_rms 0.557 # Attachment 'Structure 1 CsCe2F8F(H2O).cif' data_structure1 _database_code_depnum_ccdc_archive 'CCDC 737295' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H2 Ce2 Cs F9 O' _chemical_formula_weight 602.17 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.4579(5) _cell_length_b 6.9826(2) _cell_length_c 8.5656(2) _cell_angle_alpha 90.00 _cell_angle_beta 117.938(2) _cell_angle_gamma 90.00 _cell_volume 816.79(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6752 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.897 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 15.513 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3061 _exptl_absorpt_correction_T_max 0.7467 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4230 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 24.98 _reflns_number_total 719 _reflns_number_gt 683 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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^ > 2\s(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. An isotropic thermal restraint was used to reduce the prolate nature of the oxygen temperature factor. The O1/F5 site is split based on charge balance backed up by IR and EDX analysis. The hydrogen atom shave been included in the formula, but not the refinement. ; _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^)+(0.0681P)^2^+9.3573P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 719 _refine_ls_number_parameters 60 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0310 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.1047 _refine_ls_wR_factor_gt 0.1013 _refine_ls_goodness_of_fit_ref 1.185 _refine_ls_restrained_S_all 1.185 _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 F1 F 0.3397(3) 0.8954(5) 0.3631(6) 0.0084(10) Uani 1 1 d . . . F2 F 0.3306(3) 1.2809(6) 0.2760(5) 0.0093(9) Uani 1 1 d . . . Cs1 Cs 0.5000 1.10479(10) 0.2500 0.0122(3) Uani 1 2 d S . . Ce1 Ce 0.21372(3) 1.09670(6) 0.29446(6) 0.0063(3) Uani 1 1 d . . . F3 F 0.3343(3) 1.1807(6) 0.5688(5) 0.0096(9) Uani 1 1 d . . . F4 F 0.1851(3) 1.0489(7) 0.0131(5) 0.0105(9) Uani 1 1 d . . . O1 O 0.0465(5) 1.0894(8) 0.1517(8) 0.0169(14) Uani 0.50 1 d P . . F5 F 0.0465(5) 1.0894(8) 0.1517(8) 0.0169(14) Uani 0.50 1 d P . . 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 F1 0.010(2) 0.009(3) 0.003(2) -0.0005(15) -0.0001(18) 0.0014(16) F2 0.008(2) 0.011(2) 0.009(2) 0.0011(17) 0.0049(17) 0.0016(19) Cs1 0.0069(5) 0.0179(6) 0.0102(5) 0.000 0.0027(4) 0.000 Ce1 0.0056(4) 0.0090(4) 0.0042(4) -0.00036(13) 0.0022(3) -0.00010(14) F3 0.005(2) 0.016(3) 0.007(2) 0.0002(19) 0.0025(16) 0.0030(19) F4 0.014(2) 0.010(2) 0.007(2) -0.0015(18) 0.0042(18) -0.003(2) O1 0.014(3) 0.026(4) 0.009(3) -0.004(2) 0.005(2) -0.007(2) F5 0.014(3) 0.026(4) 0.009(3) -0.004(2) 0.005(2) -0.007(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 F1 Ce1 2.245(4) . ? F1 Ce1 2.411(4) 4_545 ? F1 Cs1 3.070(4) 5_676 ? F1 Cs1 3.386(4) . ? F2 Ce1 2.283(4) . ? F2 Ce1 2.304(4) 4 ? F2 Cs1 2.993(4) . ? Cs1 F2 2.993(4) 2_655 ? Cs1 F3 3.036(4) 6_575 ? Cs1 F3 3.036(4) 5_676 ? Cs1 F1 3.070(4) 5_676 ? Cs1 F1 3.070(4) 6_575 ? Cs1 F1 3.386(4) 2_655 ? Ce1 F4 2.262(4) . ? Ce1 F3 2.270(4) 7_576 ? Ce1 O1 2.285(6) . ? Ce1 F3 2.288(4) . ? Ce1 F2 2.304(4) 4_545 ? Ce1 F4 2.348(4) 6_576 ? Ce1 F1 2.411(4) 4 ? F3 Ce1 2.270(4) 7_576 ? F3 Cs1 3.036(4) 5_676 ? F4 Ce1 2.348(4) 6_575 ? 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 Ce1 F1 Ce1 111.56(18) . 4_545 ? Ce1 F1 Cs1 116.46(16) . 5_676 ? Ce1 F1 Cs1 119.70(15) 4_545 5_676 ? Ce1 F1 Cs1 108.42(14) . . ? Ce1 F1 Cs1 108.54(15) 4_545 . ? Cs1 F1 Cs1 88.87(11) 5_676 . ? Ce1 F2 Ce1 114.14(18) . 4 ? Ce1 F2 Cs1 121.47(17) . . ? Ce1 F2 Cs1 122.48(17) 4 . ? F2 Cs1 F2 131.49(17) 2_655 . ? F2 Cs1 F3 142.13(11) 2_655 6_575 ? F2 Cs1 F3 75.52(11) . 6_575 ? F2 Cs1 F3 75.52(11) 2_655 5_676 ? F2 Cs1 F3 142.13(11) . 5_676 ? F3 Cs1 F3 97.93(17) 6_575 5_676 ? F2 Cs1 F1 77.81(11) 2_655 5_676 ? F2 Cs1 F1 102.22(11) . 5_676 ? F3 Cs1 F1 127.76(11) 6_575 5_676 ? F3 Cs1 F1 52.19(11) 5_676 5_676 ? F2 Cs1 F1 102.22(11) 2_655 6_575 ? F2 Cs1 F1 77.81(11) . 6_575 ? F3 Cs1 F1 52.19(11) 6_575 6_575 ? F3 Cs1 F1 127.76(11) 5_676 6_575 ? F1 Cs1 F1 179.94(15) 5_676 6_575 ? F2 Cs1 F1 168.91(11) 2_655 . ? F2 Cs1 F1 51.20(11) . . ? F3 Cs1 F1 46.18(10) 6_575 . ? F3 Cs1 F1 97.21(10) 5_676 . ? F1 Cs1 F1 91.13(11) 5_676 . ? F1 Cs1 F1 88.85(11) 6_575 . ? F2 Cs1 F1 51.20(11) 2_655 2_655 ? F2 Cs1 F1 168.91(11) . 2_655 ? F3 Cs1 F1 97.21(10) 6_575 2_655 ? F3 Cs1 F1 46.18(10) 5_676 2_655 ? F1 Cs1 F1 88.85(11) 5_676 2_655 ? F1 Cs1 F1 91.13(11) 6_575 2_655 ? F1 Cs1 F1 128.85(13) . 2_655 ? F2 Cs1 F4 46.16(10) 2_655 8_576 ? F2 Cs1 F4 98.23(11) . 8_576 ? F3 Cs1 F4 171.69(10) 6_575 8_576 ? F3 Cs1 F4 83.61(11) 5_676 8_576 ? F1 Cs1 F4 47.52(10) 5_676 8_576 ? F1 Cs1 F4 132.53(10) 6_575 8_576 ? F1 Cs1 F4 125.58(9) . 8_576 ? F1 Cs1 F4 89.75(9) 2_655 8_576 ? F2 Cs1 F4 98.23(11) 2_655 7_575 ? F2 Cs1 F4 46.16(10) . 7_575 ? F3 Cs1 F4 83.61(11) 6_575 7_575 ? F3 Cs1 F4 171.69(10) 5_676 7_575 ? F1 Cs1 F4 132.53(10) 5_676 7_575 ? F1 Cs1 F4 47.52(10) 6_575 7_575 ? F1 Cs1 F4 89.75(9) . 7_575 ? F1 Cs1 F4 125.58(9) 2_655 7_575 ? F4 Cs1 F4 96.04(14) 8_576 7_575 ? F2 Cs1 F5 47.66(13) 2_655 3 ? F2 Cs1 F5 84.81(13) . 3 ? F3 Cs1 F5 134.67(13) 6_575 3 ? F3 Cs1 F5 121.20(13) 5_676 3 ? F1 Cs1 F5 95.92(12) 5_676 3 ? F1 Cs1 F5 84.13(12) 6_575 3 ? F1 Cs1 F5 135.88(12) . 3 ? F1 Cs1 F5 94.87(12) 2_655 3 ? F4 Cs1 F5 48.54(12) 8_576 3 ? F4 Cs1 F5 54.42(12) 7_575 3 ? F2 Cs1 O1 47.66(13) 2_655 3 ? F2 Cs1 O1 84.81(13) . 3 ? F3 Cs1 O1 134.67(13) 6_575 3 ? F3 Cs1 O1 121.20(13) 5_676 3 ? F1 Cs1 O1 95.92(12) 5_676 3 ? F1 Cs1 O1 84.13(12) 6_575 3 ? F1 Cs1 O1 135.88(12) . 3 ? F1 Cs1 O1 94.87(12) 2_655 3 ? F4 Cs1 O1 48.54(12) 8_576 3 ? F4 Cs1 O1 54.42(12) 7_575 3 ? F5 Cs1 O1 0.00(6) 3 3 ? F1 Ce1 F4 84.24(16) . . ? F1 Ce1 F3 138.29(14) . 7_576 ? F4 Ce1 F3 134.64(15) . 7_576 ? F1 Ce1 F2 75.71(15) . . ? F4 Ce1 F2 77.02(15) . . ? F3 Ce1 F2 96.36(15) 7_576 . ? F1 Ce1 O1 138.72(17) . . ? F4 Ce1 O1 79.57(19) . . ? F3 Ce1 O1 74.33(18) 7_576 . ? F2 Ce1 O1 135.20(18) . . ? F1 Ce1 F3 72.68(15) . . ? F4 Ce1 F3 142.26(15) . . ? F3 Ce1 F3 66.44(17) 7_576 . ? F2 Ce1 F3 68.69(15) . . ? O1 Ce1 F3 136.74(18) . . ? F1 Ce1 F2 65.47(15) . 4_545 ? F4 Ce1 F2 72.19(15) . 4_545 ? F3 Ce1 F2 131.40(15) 7_576 4_545 ? F2 Ce1 F2 131.99(11) . 4_545 ? O1 Ce1 F2 73.45(18) . 4_545 ? F3 Ce1 F2 120.90(15) . 4_545 ? F1 Ce1 F4 89.11(15) . 6_576 ? F4 Ce1 F4 140.35(11) . 6_576 ? F3 Ce1 F4 69.86(15) 7_576 6_576 ? F2 Ce1 F4 138.62(15) . 6_576 ? O1 Ce1 F4 80.11(18) . 6_576 ? F3 Ce1 F4 70.07(15) . 6_576 ? F2 Ce1 F4 69.53(15) 4_545 6_576 ? F1 Ce1 F1 135.72(7) . 4 ? F4 Ce1 F1 71.71(16) . 4 ? F3 Ce1 F1 65.63(15) 7_576 4 ? F2 Ce1 F1 63.16(15) . 4 ? O1 Ce1 F1 73.43(17) . 4 ? F3 Ce1 F1 104.70(15) . 4 ? F2 Ce1 F1 134.39(14) 4_545 4 ? F4 Ce1 F1 132.70(15) 6_576 4 ? F1 Ce1 Ce1 105.41(11) . 7_576 ? F4 Ce1 Ce1 153.23(12) . 7_576 ? F3 Ce1 Ce1 33.37(10) 7_576 7_576 ? F2 Ce1 Ce1 81.25(10) . 7_576 ? O1 Ce1 Ce1 106.04(15) . 7_576 ? F3 Ce1 Ce1 33.07(10) . 7_576 ? F2 Ce1 Ce1 134.58(10) 4_545 7_576 ? F4 Ce1 Ce1 65.82(12) 6_576 7_576 ? F1 Ce1 Ce1 84.65(10) 4 7_576 ? F1 Ce1 Ce1 108.79(11) . 4 ? F4 Ce1 Ce1 81.53(12) . 4 ? F3 Ce1 Ce1 71.16(11) 7_576 4 ? F2 Ce1 Ce1 33.10(11) . 4 ? O1 Ce1 Ce1 106.01(14) . 4 ? F3 Ce1 Ce1 78.36(11) . 4 ? F2 Ce1 Ce1 153.43(10) 4_545 4 ? F4 Ce1 Ce1 137.02(12) 6_576 4 ? F1 Ce1 Ce1 32.84(10) 4 4 ? Ce1 Ce1 Ce1 71.741(12) 7_576 4 ? Ce1 F3 Ce1 113.56(17) 7_576 . ? Ce1 F3 Cs1 125.96(15) 7_576 5_676 ? Ce1 F3 Cs1 116.28(16) . 5_676 ? Ce1 F4 Ce1 153.9(2) . 6_575 ? Ce1 F4 Cs1 105.56(15) . 7_575 ? Ce1 F4 Cs1 100.51(13) 6_575 7_575 ? Ce1 O1 Cs1 101.16(18) . 3_445 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.750 _refine_diff_density_min -1.694 _refine_diff_density_rms 0.504 # Attachment 'Structure 5 NH4CeF2AsO4.cif' data_structure5 _database_code_depnum_ccdc_archive 'CCDC 737296' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H4 As Ce F2 N O4' _chemical_formula_weight 335.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 6.7758(2) _cell_length_b 6.0181(2) _cell_length_c 7.1315(2) _cell_angle_alpha 90.00 _cell_angle_beta 113.832(2) _cell_angle_gamma 90.00 _cell_volume 266.009(14) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3710 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 33.14 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.183 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 304 _exptl_absorpt_coefficient_mu 14.718 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1568 _exptl_absorpt_correction_T_max 0.3208 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5124 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 33.16 _reflns_number_total 1096 _reflns_number_gt 1068 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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^ > 2\s(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. The hydrogen atoms have been included in the formula, but not the refinement. ; _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^)+(0.0502P)^2^+0.3232P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1096 _refine_ls_number_parameters 49 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0282 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0978 _refine_ls_wR_factor_gt 0.0973 _refine_ls_goodness_of_fit_ref 1.339 _refine_ls_restrained_S_all 1.338 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ce1 Ce 0.38194(5) 0.2500 0.30323(4) 0.00225(12) Uani 1 2 d S . . As1 As -0.22807(9) 0.2500 0.04132(8) 0.00246(15) Uani 1 2 d S . . F1 F 0.6607(4) -0.0040(4) 0.4575(3) 0.0069(4) Uani 1 1 d . . . O1 O -0.0010(7) 0.2500 0.2596(6) 0.0061(7) Uani 1 2 d SU . . O2 O -0.2279(5) 0.0258(4) -0.1018(4) 0.0082(5) Uani 1 1 d . . . O3 O -0.4492(7) 0.2500 0.0904(6) 0.0075(7) Uani 1 2 d S . . N1 N 1.0545(8) 0.2500 0.6800(7) 0.0067(8) 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 Ce1 0.00214(17) 0.00238(19) 0.00172(18) 0.000 0.00026(12) 0.000 As1 0.0023(3) 0.0030(3) 0.0019(3) 0.000 0.0007(2) 0.000 F1 0.0056(10) 0.0097(10) 0.0063(10) 0.0042(8) 0.0034(8) 0.0034(8) O1 0.0060(10) 0.0069(10) 0.0047(10) 0.000 0.0014(8) 0.000 O2 0.0057(12) 0.0087(12) 0.0099(12) -0.0051(10) 0.0028(10) -0.0004(10) O3 0.0055(17) 0.0098(17) 0.0094(17) 0.000 0.0054(15) 0.000 N1 0.006(2) 0.009(2) 0.004(2) 0.000 0.0001(17) 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 O2 2.167(3) 3 ? Ce1 O2 2.167(3) 2 ? Ce1 O3 2.240(4) 1_655 ? Ce1 F1 2.331(2) 4_565 ? Ce1 F1 2.331(2) . ? Ce1 F1 2.363(2) 2_656 ? Ce1 F1 2.363(2) 3_656 ? Ce1 O1 2.486(4) . ? Ce1 Ce1 3.9827(4) 3_666 ? Ce1 Ce1 3.9827(4) 3_656 ? As1 O3 1.671(4) . ? As1 O1 1.689(4) . ? As1 O2 1.692(3) . ? As1 O2 1.692(3) 4_565 ? F1 Ce1 2.363(2) 3_656 ? O2 Ce1 2.167(3) 3 ? O3 Ce1 2.240(4) 1_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 O2 Ce1 O2 99.99(16) 3 2 ? O2 Ce1 O3 77.99(10) 3 1_655 ? O2 Ce1 O3 77.99(10) 2 1_655 ? O2 Ce1 F1 153.70(9) 3 4_565 ? O2 Ce1 F1 83.80(10) 2 4_565 ? O3 Ce1 F1 77.39(10) 1_655 4_565 ? O2 Ce1 F1 83.80(10) 3 . ? O2 Ce1 F1 153.70(9) 2 . ? O3 Ce1 F1 77.39(10) 1_655 . ? F1 Ce1 F1 81.95(12) 4_565 . ? O2 Ce1 F1 142.35(9) 3 2_656 ? O2 Ce1 F1 80.33(9) 2 2_656 ? O3 Ce1 F1 137.24(7) 1_655 2_656 ? F1 Ce1 F1 63.92(8) 4_565 2_656 ? F1 Ce1 F1 112.46(4) . 2_656 ? O2 Ce1 F1 80.33(9) 3 3_656 ? O2 Ce1 F1 142.35(9) 2 3_656 ? O3 Ce1 F1 137.24(7) 1_655 3_656 ? F1 Ce1 F1 112.46(4) 4_565 3_656 ? F1 Ce1 F1 63.92(8) . 3_656 ? F1 Ce1 F1 77.58(11) 2_656 3_656 ? O2 Ce1 O1 73.63(9) 3 . ? O2 Ce1 O1 73.63(9) 2 . ? O3 Ce1 O1 135.11(15) 1_655 . ? F1 Ce1 O1 131.66(7) 4_565 . ? F1 Ce1 O1 131.66(7) . . ? F1 Ce1 O1 70.40(9) 2_656 . ? F1 Ce1 O1 70.40(9) 3_656 . ? O2 Ce1 Ce1 174.00(7) 3 3_666 ? O2 Ce1 Ce1 80.62(8) 2 3_666 ? O3 Ce1 Ce1 107.93(7) 1_655 3_666 ? F1 Ce1 Ce1 32.20(5) 4_565 3_666 ? F1 Ce1 Ce1 98.32(6) . 3_666 ? F1 Ce1 Ce1 31.72(5) 2_656 3_666 ? F1 Ce1 Ce1 95.51(6) 3_656 3_666 ? O1 Ce1 Ce1 100.96(6) . 3_666 ? O2 Ce1 Ce1 80.62(8) 3 3_656 ? O2 Ce1 Ce1 174.00(7) 2 3_656 ? O3 Ce1 Ce1 107.93(7) 1_655 3_656 ? F1 Ce1 Ce1 98.32(6) 4_565 3_656 ? F1 Ce1 Ce1 32.20(5) . 3_656 ? F1 Ce1 Ce1 95.51(6) 2_656 3_656 ? F1 Ce1 Ce1 31.72(5) 3_656 3_656 ? O1 Ce1 Ce1 100.96(6) . 3_656 ? Ce1 Ce1 Ce1 98.142(12) 3_666 3_656 ? O3 As1 O1 111.5(2) . . ? O3 As1 O2 110.22(12) . . ? O1 As1 O2 109.48(12) . . ? O3 As1 O2 110.22(12) . 4_565 ? O1 As1 O2 109.48(12) . 4_565 ? O2 As1 O2 105.74(19) . 4_565 ? Ce1 F1 Ce1 116.08(8) . 3_656 ? As1 O1 Ce1 129.15(18) . . ? As1 O2 Ce1 153.25(17) . 3 ? As1 O3 Ce1 152.7(3) . 1_455 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 33.16 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.553 _refine_diff_density_min -2.975 _refine_diff_density_rms 0.721