#------------------------------------------------------------------------------ #$Date: 2020-02-04 22:10:48 +0200 (Tue, 04 Feb 2020) $ #$Revision: 247622 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/56/7125640.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7125640 loop_ _publ_author_name 'Zhang, Shan' 'Lu, Ying' 'Sun, Xiu-Wei' 'Li, Zhuo' 'Dang, Tian-Yi' 'Zhang, Zhong' 'Tian, Hong-Rui' 'Liu, Shu-Xia' _publ_section_title ; Purely inorganic frameworks based on polyoxometalate clusters with abundant phosphate groups: single-crystal to single-crystal structural transformation and remarkable proton conduction. ; _journal_issue 3 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 391 _journal_page_last 394 _journal_paper_doi 10.1039/c9cc08696j _journal_volume 56 _journal_year 2020 _chemical_formula_moiety '0.5(Fe80 Mo192 Na64 O1170.86 P136), 40(O)' _chemical_formula_sum 'Fe40 Mo96 Na32 O625.43 P68' _chemical_formula_weight 24292.76 _space_group_crystal_system tetragonal _space_group_IT_number 142 _space_group_name_Hall '-I 4bd 2c' _space_group_name_H-M_alt 'I 41/a c d :2' _atom_sites_solution_primary iterative _audit_creation_date 2019-04-01 _audit_creation_method ; Olex2 1.2-beta (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-09-25 deposited with the CCDC. 2019-11-27 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 27.3577(9) _cell_length_b 27.3577(9) _cell_length_c 38.0332(12) _cell_measurement_reflns_used 9819 _cell_measurement_temperature 100 _cell_measurement_theta_max 25.04 _cell_measurement_theta_min 2.31 _cell_volume 28465.7(16) _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve (Bourhis et al., 2015)' _diffrn_ambient_temperature 100.0 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0683 _diffrn_reflns_av_unetI/netI 0.0300 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_number 79867 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.061 _diffrn_reflns_theta_max 25.061 _diffrn_reflns_theta_min 2.609 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.369 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 2.834 _exptl_crystal_description block _exptl_crystal_F_000 22895 _refine_diff_density_max 1.171 _refine_diff_density_min -1.214 _refine_diff_density_rms 0.181 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 538 _refine_ls_number_reflns 6311 _refine_ls_number_restraints 54 _refine_ls_restrained_S_all 1.085 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0388 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+762.9777P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0968 _refine_ls_wR_factor_ref 0.1064 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5100 _reflns_number_total 6311 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc08696j2.cif _cod_data_source_block 1 _cod_depositor_comments 'Adding full bibliography for 7125640--7125641.cif.' _cod_original_cell_volume 28466(2) _cod_original_sg_symbol_H-M 'I 41/a c d' _cod_database_code 7125640 _shelx_shelxl_version_number 2017/1 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _olex2_refinement_description ; 1. Uiso/Uaniso restraints and constraints Uanis(O8W) \\sim Ueq, Uanis(O4W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O5W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O6W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O9W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O3W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O2W) \\sim Ueq, Uanis(O6W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O3W) \\sim Ueq, Uanis(O3WA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O2W) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 Uanis(O9WA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 2. Others Fixed Sof: O6W(0.5) O7W(0.5) O5W(0.125) O4W(0.125) O8W(0.125) Na3(0.5) O10W(0.25) O9W(0.5) O3W(0.25) O3WA(0.25) O9WA(0.5) ; _shelx_res_file ; TITL w_a.res in I4(1)/acd 1.res created by SHELXL-2017/1 at 16:57:35 on 01-Apr-2019 REM Old TITL w in I4(1)/acd REM SHELXT solution in I4(1)/acd REM R1 0.118, Rweak 0.004, Alpha 0.023, Orientation as input REM Formula found by SHELXT: C34 O122 P8 S9 Fe10 Mo24 CELL 0.71073 27.3577 27.3577 38.0332 90 90 90 ZERR 2 0.0009 0.0009 0.0012 0 0 0 LATT 2 SYMM 0.5-X,-Y,0.5+Z SYMM 0.25-Y,0.75+X,0.25+Z SYMM 0.25+Y,0.25-X,0.75+Z SYMM 0.5-X,+Y,-Z SYMM +X,-Y,0.5-Z SYMM 0.25+Y,0.75+X,0.75-Z SYMM 0.25-Y,0.25-X,0.25-Z SFAC Fe Mo Na O P UNIT 80 192 64 1250.86 136 EQIV $1 1-X,0.5-Y,+Z EQIV $2 0.75-Y,-0.25+X,1.25-Z EQIV $3 0.25+Y,0.75-X,1.25-Z ISOR 0.01 0.02 O8W O4W ISOR 0.01 0.02 O5W ISOR 0.01 0.02 O6W ISOR 0.01 0.02 O9W ISOR 0.01 0.02 O3W ISOR 0.01 0.02 O2W O6W ISOR 0.01 0.02 O3W O3WA ISOR 0.005 0.01 O2W ISOR 0.01 0.02 O9WA L.S. 4 PLAN 20 TEMP -173.15 FREE Mo5 Na1 FREE P2 Na3 FREE Fe3 Na3 FREE P1 Na1_$1 FREE P1 Na1_$3 FREE P1 Na1_$2 FREE P1 Na1 FREE P3 Na1 FREE P3 Na2_$1 FREE P3 Na2 FREE Fe1 Na1 list 4 conf fmap 2.0 acta OMIT 0 0 8 OMIT 2 2 4 OMIT 1 2 5 OMIT 1 4 5 OMIT 0 6 0 OMIT 1 3 2 OMIT 0 2 6 REM REM REM WGHT 0.042200 762.977661 FVAR 0.01967 MO1 2 0.282795 0.144052 0.585990 11.00000 0.01145 0.01372 = 0.01920 -0.00234 -0.00162 -0.00110 MO2 2 0.319756 0.096802 0.532950 11.00000 0.00925 0.01138 = 0.02197 -0.00197 -0.00100 0.00018 MO4 2 0.372335 0.256066 0.463151 11.00000 0.01490 0.01535 = 0.01692 0.00098 -0.00494 0.00025 MO3 2 0.371869 0.161841 0.463494 11.00000 0.01477 0.01457 = 0.01635 -0.00097 -0.00407 0.00315 MO5 2 0.319679 0.319810 0.527776 11.00000 0.01156 0.01334 = 0.02854 -0.00101 -0.00466 0.00135 MO6 2 0.272849 0.266246 0.586373 11.00000 0.01396 0.01917 = 0.02187 -0.00339 -0.00407 0.00354 FE2 1 0.250000 0.209407 0.500000 10.50000 0.01354 0.01486 = 0.02201 0.00000 -0.00408 0.00000 FE1 1 0.518632 0.339157 0.567416 11.00000 0.00876 0.01106 = 0.01351 0.00013 0.00081 0.00000 FE3 1 0.456846 0.460830 0.505521 11.00000 0.02865 0.01703 = 0.02887 0.00300 -0.00153 0.00081 P1 5 0.500000 0.250000 0.625000 10.25000 0.01151 0.01151 = 0.00963 0.00000 0.00000 0.00000 P4 5 0.375595 0.207094 0.546148 11.00000 0.00828 0.00876 = 0.01684 -0.00005 -0.00225 0.00041 P2 5 0.566544 0.419629 0.508767 11.00000 0.00962 0.00982 = 0.01676 0.00155 0.00136 0.00266 P5 5 0.312806 0.209524 0.657729 11.00000 0.01269 0.01382 = 0.01719 -0.00228 0.00237 -0.00311 P3 5 0.434621 0.341592 0.507522 11.00000 0.01248 0.01072 = 0.01795 0.00247 -0.00325 -0.00186 NA1 3 0.412300 0.313720 0.588090 11.00000 0.01606 0.05913 = 0.03343 0.01362 -0.00212 -0.00432 NA2 3 0.500000 0.250000 0.493369 10.50000 0.03375 0.02522 = 0.08031 0.00000 0.00000 0.00956 O25 4 0.229645 0.149118 0.465125 11.00000 0.01584 0.01802 = 0.02046 0.00304 -0.00210 -0.00162 O23 4 0.318636 0.209085 0.470837 11.00000 0.01853 0.00998 = 0.02411 -0.00235 -0.00731 0.00269 O19 4 0.270557 0.268515 0.534960 11.00000 0.01292 0.01970 = 0.01805 -0.00219 -0.00392 -0.00401 O26 4 0.320900 0.107628 0.478468 11.00000 0.01258 0.01410 = 0.02267 -0.00372 -0.00249 -0.00039 O22 4 0.367844 0.161756 0.522372 11.00000 0.01214 0.00982 = 0.01673 -0.00472 -0.00271 -0.00135 O21 4 0.335174 0.206772 0.574391 11.00000 0.01375 0.01351 = 0.01899 -0.00221 0.00214 -0.00104 O30 4 0.342103 0.105142 0.581136 11.00000 0.01442 0.01354 = 0.02233 0.00358 -0.00126 0.00096 O5 4 0.534090 0.463791 0.499107 11.00000 0.01155 0.00887 = 0.02680 -0.00022 -0.00268 0.00313 O18 4 0.369702 0.253260 0.523592 11.00000 0.01293 0.01213 = 0.01800 0.00022 -0.00258 0.00142 O2 4 0.464213 0.383772 0.584233 11.00000 0.01340 0.01526 = 0.02311 -0.00662 0.00189 0.00212 O29 4 0.384253 0.059863 0.522518 11.00000 0.00807 0.01092 = 0.02889 0.00069 0.00284 0.00167 O1 4 0.490683 0.295179 0.602383 11.00000 0.01275 0.01574 = 0.01999 0.00791 0.00190 0.00449 O32 4 0.242314 0.206918 0.589206 11.00000 0.01083 0.02104 = 0.01875 -0.00492 0.00089 0.00100 O10 4 0.424835 0.307947 0.476038 11.00000 0.01837 0.02456 = 0.01950 -0.00063 0.00092 -0.00612 O15 4 0.324892 0.309476 0.480192 11.00000 0.01819 0.01495 = 0.02281 0.00076 -0.00541 0.00144 O3 4 0.573171 0.293082 0.561592 11.00000 0.00978 0.01376 = 0.02608 0.00050 0.00892 0.00047 O8 4 0.471678 0.315352 0.530748 11.00000 0.01854 0.00903 = 0.01819 -0.00082 -0.00566 0.00222 O11 4 0.386444 0.349738 0.529071 11.00000 0.01119 0.01588 = 0.02320 -0.00125 -0.00047 -0.00195 O12 4 0.377076 0.315965 0.644535 11.00000 0.02298 0.01611 = 0.02092 -0.00145 -0.00318 0.00319 O17 4 0.423815 0.208942 0.469464 11.00000 0.01625 0.01771 = 0.02060 0.00601 -0.00239 0.00121 O27 4 0.424038 0.109301 0.474894 11.00000 0.02046 0.01615 = 0.01568 0.00301 0.00308 0.00817 O13 4 0.328177 0.308189 0.578292 11.00000 0.01874 0.01148 = 0.02430 -0.00252 0.00016 0.00135 O4 4 0.542260 0.389866 0.536458 11.00000 0.01535 0.01747 = 0.02392 0.00546 0.00190 0.00046 O33 4 0.304033 0.162989 0.636177 11.00000 0.02410 0.01692 = 0.02239 -0.00623 -0.00693 -0.00444 O34 4 0.297791 0.255426 0.635845 11.00000 0.02109 0.01498 = 0.02697 -0.00047 -0.00729 0.00217 O7 4 0.452548 0.390358 0.494041 11.00000 0.02100 0.01218 = 0.03623 0.01072 -0.00042 -0.00184 O20 4 0.228358 0.305702 0.596567 11.00000 0.01717 0.02663 = 0.03690 -0.00948 -0.00195 0.00800 O28 4 0.285495 0.046114 0.533738 11.00000 0.01935 0.01718 = 0.03724 -0.00274 0.00064 -0.00540 O24 4 0.369471 0.149540 0.420096 11.00000 0.03304 0.02764 = 0.01880 -0.00361 -0.00764 0.00672 O9 4 0.282195 0.208209 0.691300 11.00000 0.03913 0.03391 = 0.03073 -0.00255 0.02482 -0.00906 O14 4 0.285829 0.370843 0.528925 11.00000 0.02146 0.01852 = 0.04253 -0.00124 -0.00606 0.00533 O31 4 0.239374 0.103954 0.598354 11.00000 0.01628 0.02417 = 0.03281 -0.00118 0.00281 -0.00653 O16 4 0.371176 0.267872 0.419893 11.00000 0.03490 0.02839 = 0.01758 0.00225 -0.00655 -0.00515 O1W 4 0.379923 0.466626 0.502887 11.00000 0.04952 0.04271 = 0.07450 -0.00476 -0.00924 0.00310 O6 4 0.457998 0.467918 0.446781 11.00000 0.07038 0.03752 = 0.04909 -0.00162 0.01438 -0.01037 O2W 4 0.556136 0.423587 0.396295 0.96427 0.10887 0.08947 = 0.07791 0.02706 0.00125 0.02764 O6W 4 0.356074 0.530199 0.570731 10.50000 0.09229 0.04783 = 0.04606 0.04040 0.02171 0.02752 O7W 4 0.326826 0.412043 0.452740 10.50000 0.13941 0.06642 = 0.11124 0.06569 -0.08251 -0.07834 O5W 4 0.250000 0.460885 0.500000 10.12500 0.07234 0.03851 = 0.07109 0.00000 0.01313 0.00000 O4W 4 0.500000 0.250000 0.420350 10.12500 0.05515 0.07320 = 0.05742 0.00000 0.00000 -0.00263 O8W 4 0.449212 0.199212 0.375000 10.12500 0.08459 0.08459 = 0.09063 -0.02030 0.02030 -0.00236 NA3 3 0.500816 0.393651 0.438155 10.50000 0.05787 0.22451 = 0.05016 0.05682 0.01818 0.03336 O10W 4 0.341479 0.091479 0.375000 10.25000 0.05280 0.05280 = 0.06666 -0.03159 0.03159 -0.01349 PART 1 O9W 4 0.245460 0.374926 0.658655 10.50000 0.13287 0.12318 = 0.09047 -0.03702 -0.03244 -0.01436 O3W 4 0.459714 0.358101 0.409663 10.25000 0.08980 0.09689 = 0.05307 0.02642 0.01395 -0.02550 PART 0 PART 2 O3WA 4 0.423467 0.380696 0.398687 10.25000 0.11933 0.10083 = 0.09972 -0.00734 0.04965 -0.01139 O9WA 4 0.287727 0.409501 0.610076 10.50000 0.20533 0.20760 = 0.21758 -0.05588 -0.06611 -0.02253 HKLF 4 REM w_a.res in I4(1)/acd REM R1 = 0.0388 for 5100 Fo > 4sig(Fo) and 0.0574 for all 6311 data REM 538 parameters refined using 54 restraints END WGHT 0.0422 763.0184 REM Highest difference peak 1.171, deepest hole -1.214, 1-sigma level 0.181 Q1 1 0.4406 0.2316 0.3486 11.00000 0.05 1.17 Q2 1 0.2670 0.4825 0.5861 11.00000 0.05 1.11 Q3 1 0.2706 0.4673 0.5628 11.00000 0.05 1.05 Q4 1 0.1976 0.3734 0.6526 11.00000 0.05 1.04 Q5 1 0.5000 0.2500 0.3750 10.25000 0.05 0.92 Q6 1 0.4315 0.4765 0.4307 11.00000 0.05 0.90 Q7 1 0.3185 0.4024 0.4353 11.00000 0.05 0.87 Q8 1 0.3808 0.5474 0.5850 11.00000 0.05 0.84 Q9 1 0.3472 0.2993 0.6358 11.00000 0.05 0.82 Q10 1 0.3395 0.5479 0.5753 11.00000 0.05 0.82 Q11 1 0.5038 0.3532 0.4187 11.00000 0.05 0.82 Q12 1 0.2603 0.4075 0.6365 11.00000 0.05 0.81 Q13 1 0.3259 0.5197 0.5675 11.00000 0.05 0.81 Q14 1 0.3232 0.4100 0.4654 11.00000 0.05 0.78 Q15 1 0.3005 0.4329 0.4528 11.00000 0.05 0.77 Q16 1 0.3318 0.5377 0.5737 11.00000 0.05 0.77 Q17 1 0.4426 0.3782 0.4144 11.00000 0.05 0.74 Q18 1 0.3772 0.5327 0.5653 11.00000 0.05 0.72 Q19 1 0.3313 0.4483 0.5701 11.00000 0.05 0.70 Q20 1 0.3025 0.4477 0.4680 11.00000 0.05 0.69 ; _shelx_res_checksum 78220 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+1/4, x+3/4, z+1/4' 'y+1/4, -x+1/4, z+3/4' '-x+1/2, y, -z' 'x, -y, -z+1/2' 'y+1/4, x+3/4, -z+3/4' '-y+1/4, -x+1/4, -z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+3/4, x+5/4, z+3/4' 'y+3/4, -x+3/4, z+5/4' '-x+1, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1' 'y+3/4, x+5/4, -z+5/4' '-y+3/4, -x+3/4, -z+3/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-1/4, -x-3/4, -z-1/4' '-y-1/4, x-1/4, -z-3/4' 'x-1/2, -y, z' '-x, y, z-1/2' '-y-1/4, -x-3/4, z-3/4' 'y-1/4, x-1/4, z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y+1/4, -x-1/4, -z+1/4' '-y+1/4, x+1/4, -z-1/4' 'x, -y+1/2, z+1/2' '-x+1/2, y+1/2, z' '-y+1/4, -x-1/4, z-1/4' 'y+1/4, x+1/4, z+1/4' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.28279(2) 0.14405(2) 0.58599(2) 0.01479(16) Uani 1 1 d . . . . . Mo2 Mo 0.31976(2) 0.09680(2) 0.53295(2) 0.01420(16) Uani 1 1 d . . . . . Mo4 Mo 0.37234(2) 0.25607(2) 0.46315(2) 0.01572(16) Uani 1 1 d . . . . . Mo3 Mo 0.37187(2) 0.16184(2) 0.46349(2) 0.01523(16) Uani 1 1 d . . . . . Mo5 Mo 0.31968(2) 0.31981(2) 0.52778(2) 0.01781(17) Uani 1 1 d . . . . . Mo6 Mo 0.27285(2) 0.26625(3) 0.58637(2) 0.01833(17) Uani 1 1 d . . . . . Fe2 Fe 0.250000 0.20941(6) 0.500000 0.0168(3) Uani 1 2 d S T P . . Fe1 Fe 0.51863(4) 0.33916(4) 0.56742(3) 0.0111(2) Uani 1 1 d . . . . . Fe3 Fe 0.45685(5) 0.46083(4) 0.50552(3) 0.0248(3) Uani 1 1 d . . . . . P1 P 0.500000 0.250000 0.625000 0.0109(7) Uani 1 4 d S T P . . P4 P 0.37560(7) 0.20709(7) 0.54615(5) 0.0113(4) Uani 1 1 d . . . . . P2 P 0.56654(7) 0.41963(7) 0.50877(5) 0.0121(4) Uani 1 1 d . . . . . P5 P 0.31281(7) 0.20952(7) 0.65773(5) 0.0146(4) Uani 1 1 d . . . . . P3 P 0.43462(7) 0.34159(7) 0.50752(5) 0.0137(4) Uani 1 1 d . . . . . Na1 Na 0.41230(12) 0.31372(15) 0.58809(9) 0.0362(9) Uani 1 1 d . . . . . Na2 Na 0.500000 0.250000 0.49337(17) 0.0464(15) Uani 1 2 d S T P . . O25 O 0.22965(19) 0.14912(19) 0.46513(14) 0.0181(12) Uani 1 1 d . . . . . O23 O 0.31864(19) 0.20909(18) 0.47084(14) 0.0175(12) Uani 1 1 d . . . . . O19 O 0.27056(18) 0.26852(19) 0.53496(13) 0.0169(11) Uani 1 1 d . . . . . O26 O 0.32090(18) 0.10763(19) 0.47847(14) 0.0164(11) Uani 1 1 d . . . . . O22 O 0.36784(18) 0.16176(18) 0.52237(13) 0.0129(11) Uani 1 1 d . . . . . O21 O 0.33517(18) 0.20677(18) 0.57439(13) 0.0154(11) Uani 1 1 d . . . . . O30 O 0.34210(19) 0.10514(18) 0.58114(13) 0.0168(11) Uani 1 1 d . . . . . O5 O 0.53409(18) 0.46379(18) 0.49911(14) 0.0157(11) Uani 1 1 d . . . . . O18 O 0.36970(18) 0.25326(18) 0.52359(13) 0.0144(11) Uani 1 1 d . . . . . O2 O 0.46421(18) 0.38377(19) 0.58423(14) 0.0173(12) Uani 1 1 d . . . . . O29 O 0.38425(18) 0.05986(18) 0.52252(14) 0.0160(11) Uani 1 1 d . . . . . O1 O 0.49068(18) 0.29518(18) 0.60238(13) 0.0162(11) Uani 1 1 d . . . . . O32 O 0.24231(18) 0.20692(19) 0.58921(13) 0.0169(11) Uani 1 1 d . . . . . O10 O 0.4248(2) 0.3079(2) 0.47604(14) 0.0208(12) Uani 1 1 d . . . . . O15 O 0.32489(19) 0.30948(19) 0.48019(14) 0.0187(12) Uani 1 1 d . . . . . O3 O 0.57317(18) 0.29308(18) 0.56159(14) 0.0165(11) Uani 1 1 d . . . . . O8 O 0.47168(19) 0.31535(18) 0.53075(13) 0.0153(11) Uani 1 1 d . . . . . O11 O 0.38644(18) 0.34974(19) 0.52907(13) 0.0168(11) Uani 1 1 d . . . . . O12 O 0.3771(2) 0.31596(19) 0.64454(14) 0.0200(12) Uani 1 1 d . . . . . O17 O 0.42381(19) 0.20894(19) 0.46946(14) 0.0182(12) Uani 1 1 d . . . . . O27 O 0.42404(19) 0.10930(19) 0.47489(13) 0.0174(12) Uani 1 1 d . . . . . O13 O 0.32818(19) 0.30819(19) 0.57829(14) 0.0182(12) Uani 1 1 d . . . . . O4 O 0.54226(19) 0.38987(19) 0.53646(14) 0.0189(12) Uani 1 1 d . . . . . O33 O 0.3040(2) 0.1630(2) 0.63618(14) 0.0211(12) Uani 1 1 d . . . . . O34 O 0.2978(2) 0.2554(2) 0.63584(14) 0.0210(12) Uani 1 1 d . . . . . O7 O 0.4525(2) 0.39036(19) 0.49404(15) 0.0231(13) Uani 1 1 d . . . . . O20 O 0.2284(2) 0.3057(2) 0.59657(16) 0.0269(14) Uani 1 1 d . . . . . O28 O 0.2855(2) 0.0461(2) 0.53374(15) 0.0246(13) Uani 1 1 d . . . . . O24 O 0.3695(2) 0.1495(2) 0.42010(14) 0.0265(14) Uani 1 1 d . . . . . O9 O 0.2822(2) 0.2082(2) 0.69130(16) 0.0346(16) Uani 1 1 d . . . . . O14 O 0.2858(2) 0.3708(2) 0.52893(16) 0.0275(14) Uani 1 1 d . . . . . O31 O 0.2394(2) 0.1040(2) 0.59835(15) 0.0244(13) Uani 1 1 d . . . . . O16 O 0.3712(2) 0.2679(2) 0.41989(14) 0.0270(14) Uani 1 1 d . . . . . O1W O 0.3799(3) 0.4666(3) 0.5029(2) 0.056(2) Uani 1 1 d . . . . . O6 O 0.4580(3) 0.4679(3) 0.4468(2) 0.052(2) Uani 1 1 d . . . . . O2W O 0.5561(4) 0.4236(4) 0.3963(3) 0.092(5) Uani 0.96(3) 1 d . U . B . O6W O 0.3561(7) 0.5302(6) 0.5707(4) 0.062(5) Uani 0.5 1 d . U . . . O7W O 0.3268(8) 0.4120(7) 0.4527(6) 0.106(9) Uani 0.5 1 d . . . . . O5W O 0.250000 0.4609(16) 0.500000 0.061(12) Uani 0.25 2 d S TU P . . O4W O 0.500000 0.250000 0.4203(12) 0.062(12) Uani 0.25 2 d S TU P . . O8W O 0.4492(15) 0.1992(15) 0.375000 0.087(15) Uani 0.25 2 d S TU P . . Na3 Na 0.5008(4) 0.3937(7) 0.4382(3) 0.111(6) Uani 0.5 1 d . . . . . O10W O 0.3415(5) 0.0915(5) 0.375000 0.057(6) Uani 0.5 2 d S T P . . O9W O 0.2455(10) 0.3749(9) 0.6587(6) 0.116(8) Uani 0.5 1 d . U . A 1 O3W O 0.4597(16) 0.3581(16) 0.4097(10) 0.080(11) Uani 0.25 1 d . U . B 1 O3WA O 0.423(2) 0.3807(18) 0.3987(13) 0.107(15) Uani 0.25 1 d . U . B 2 O9WA O 0.2877(15) 0.4095(15) 0.6101(11) 0.210(17) Uani 0.5 1 d . U . C 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 Mo1 0.0115(3) 0.0137(3) 0.0192(3) -0.0023(3) -0.0016(3) -0.0011(3) Mo2 0.0093(3) 0.0114(3) 0.0220(3) -0.0020(3) -0.0010(3) 0.0002(2) Mo4 0.0149(3) 0.0154(4) 0.0169(3) 0.0010(3) -0.0049(3) 0.0003(3) Mo3 0.0148(3) 0.0146(3) 0.0164(3) -0.0010(3) -0.0041(3) 0.0031(3) Mo5 0.0116(3) 0.0133(4) 0.0285(4) -0.0010(3) -0.0047(3) 0.0014(3) Mo6 0.0140(3) 0.0192(4) 0.0219(4) -0.0034(3) -0.0041(3) 0.0035(3) Fe2 0.0135(8) 0.0149(8) 0.0220(8) 0.000 -0.0041(6) 0.000 Fe1 0.0088(5) 0.0111(5) 0.0135(5) 0.0001(4) 0.0008(4) 0.0000(4) Fe3 0.0286(7) 0.0170(6) 0.0289(7) 0.0030(5) -0.0015(5) 0.0008(5) P1 0.0115(11) 0.0115(11) 0.0096(17) 0.000 0.000 0.000 P4 0.0083(9) 0.0088(9) 0.0168(9) 0.0000(7) -0.0022(7) 0.0004(7) P2 0.0096(9) 0.0098(9) 0.0168(10) 0.0015(7) 0.0014(8) 0.0027(7) P5 0.0127(10) 0.0138(10) 0.0172(10) -0.0023(8) 0.0024(8) -0.0031(8) P3 0.0125(10) 0.0107(9) 0.0179(10) 0.0025(8) -0.0032(8) -0.0019(8) Na1 0.0161(18) 0.059(3) 0.033(2) 0.0136(18) -0.0021(15) -0.0043(17) Na2 0.034(3) 0.025(3) 0.080(4) 0.000 0.000 0.010(2) O25 0.016(3) 0.018(3) 0.020(3) 0.003(2) -0.002(2) -0.002(2) O23 0.019(3) 0.010(3) 0.024(3) -0.002(2) -0.007(2) 0.003(2) O19 0.013(3) 0.020(3) 0.018(3) -0.002(2) -0.004(2) -0.004(2) O26 0.013(3) 0.014(3) 0.023(3) -0.004(2) -0.002(2) 0.000(2) O22 0.012(3) 0.010(3) 0.017(3) -0.005(2) -0.003(2) -0.001(2) O21 0.014(3) 0.014(3) 0.019(3) -0.002(2) 0.002(2) -0.001(2) O30 0.014(3) 0.014(3) 0.022(3) 0.004(2) -0.001(2) 0.001(2) O5 0.012(3) 0.009(3) 0.027(3) 0.000(2) -0.003(2) 0.003(2) O18 0.013(3) 0.012(3) 0.018(3) 0.000(2) -0.003(2) 0.001(2) O2 0.013(3) 0.015(3) 0.023(3) -0.007(2) 0.002(2) 0.002(2) O29 0.008(3) 0.011(3) 0.029(3) 0.001(2) 0.003(2) 0.002(2) O1 0.013(3) 0.016(3) 0.020(3) 0.008(2) 0.002(2) 0.004(2) O32 0.011(3) 0.021(3) 0.019(3) -0.005(2) 0.001(2) 0.001(2) O10 0.018(3) 0.025(3) 0.019(3) -0.001(2) 0.001(2) -0.006(2) O15 0.018(3) 0.015(3) 0.023(3) 0.001(2) -0.005(2) 0.001(2) O3 0.010(3) 0.014(3) 0.026(3) 0.000(2) 0.009(2) 0.000(2) O8 0.019(3) 0.009(3) 0.018(3) -0.001(2) -0.006(2) 0.002(2) O11 0.011(3) 0.016(3) 0.023(3) -0.001(2) 0.000(2) -0.002(2) O12 0.023(3) 0.016(3) 0.021(3) -0.001(2) -0.003(2) 0.003(2) O17 0.016(3) 0.018(3) 0.021(3) 0.006(2) -0.002(2) 0.001(2) O27 0.020(3) 0.016(3) 0.016(3) 0.003(2) 0.003(2) 0.008(2) O13 0.019(3) 0.011(3) 0.024(3) -0.003(2) 0.000(2) 0.001(2) O4 0.015(3) 0.017(3) 0.024(3) 0.005(2) 0.002(2) 0.000(2) O33 0.024(3) 0.017(3) 0.022(3) -0.006(2) -0.007(2) -0.004(2) O34 0.021(3) 0.015(3) 0.027(3) 0.000(2) -0.007(2) 0.002(2) O7 0.021(3) 0.012(3) 0.036(3) 0.011(2) 0.000(3) -0.002(2) O20 0.017(3) 0.027(3) 0.037(3) -0.009(3) -0.002(3) 0.008(2) O28 0.019(3) 0.017(3) 0.037(3) -0.003(3) 0.001(3) -0.005(2) O24 0.033(3) 0.028(3) 0.019(3) -0.004(2) -0.008(3) 0.007(3) O9 0.039(4) 0.034(4) 0.031(3) -0.003(3) 0.025(3) -0.009(3) O14 0.021(3) 0.019(3) 0.043(4) -0.001(3) -0.006(3) 0.005(2) O31 0.016(3) 0.024(3) 0.033(3) -0.001(3) 0.003(2) -0.007(2) O16 0.035(4) 0.028(3) 0.018(3) 0.002(2) -0.007(3) -0.005(3) O1W 0.050(5) 0.043(5) 0.074(6) -0.005(4) -0.009(4) 0.003(4) O6 0.070(6) 0.038(4) 0.049(5) -0.002(4) 0.014(4) -0.010(4) O2W 0.109(8) 0.089(8) 0.078(7) 0.027(5) 0.001(5) 0.028(6) O6W 0.092(11) 0.048(9) 0.046(8) 0.040(7) 0.022(8) 0.028(8) O7W 0.14(2) 0.066(13) 0.111(16) 0.066(12) -0.083(15) -0.078(13) O5W 0.07(2) 0.039(18) 0.071(19) 0.000 0.013(16) 0.000 O4W 0.055(15) 0.073(15) 0.057(15) 0.000 0.000 -0.003(10) O8W 0.085(17) 0.085(17) 0.09(2) -0.020(13) 0.020(13) -0.002(18) Na3 0.058(7) 0.225(17) 0.050(6) 0.057(8) 0.018(6) 0.033(9) O10W 0.053(8) 0.053(8) 0.067(15) -0.032(9) 0.032(9) -0.013(11) O9W 0.133(16) 0.123(15) 0.090(13) -0.037(12) -0.032(12) -0.014(13) O3W 0.090(19) 0.097(19) 0.053(16) 0.026(15) 0.014(15) -0.026(16) O3WA 0.12(2) 0.10(2) 0.10(2) -0.007(17) 0.050(17) -0.011(17) O9WA 0.21(2) 0.21(2) 0.22(2) -0.056(17) -0.066(17) -0.023(17) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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' 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 O25 Mo1 Mo2 48.66(15) 5_556 . O25 Mo1 O21 82.3(2) 5_556 . O25 Mo1 O32 84.7(2) 5_556 . O25 Mo1 O33 160.2(2) 5_556 . O21 Mo1 Mo2 88.83(13) . . O30 Mo1 Mo2 48.04(15) . . O30 Mo1 O25 95.1(2) . 5_556 O30 Mo1 O21 82.5(2) . . O30 Mo1 O32 156.0(2) . . O30 Mo1 O33 89.4(2) . . O32 Mo1 Mo2 132.35(15) . . O32 Mo1 O21 73.71(19) . . O32 Mo1 O33 83.5(2) . . O33 Mo1 Mo2 137.19(16) . . O33 Mo1 O21 79.2(2) . . O31 Mo1 Mo2 99.6(2) . . O31 Mo1 O25 101.5(3) . 5_556 O31 Mo1 O21 171.2(2) . . O31 Mo1 O30 104.9(3) . . O31 Mo1 O32 98.6(2) . . O31 Mo1 O33 96.0(2) . . O25 Mo2 Mo1 48.95(15) 5_556 . O25 Mo2 O26 86.8(2) 5_556 . O25 Mo2 O22 80.4(2) 5_556 . O25 Mo2 O29 161.1(2) 5_556 . O26 Mo2 Mo1 134.69(14) . . O26 Mo2 O22 72.67(19) . . O22 Mo2 Mo1 88.48(12) . . O30 Mo2 Mo1 48.17(15) . . O30 Mo2 O25 95.5(2) . 5_556 O30 Mo2 O26 155.7(2) . . O30 Mo2 O22 83.8(2) . . O30 Mo2 O29 88.3(2) . . O29 Mo2 Mo1 136.24(15) . . O29 Mo2 O26 82.3(2) . . O29 Mo2 O22 81.54(19) . . O28 Mo2 Mo1 100.4(2) . . O28 Mo2 O25 102.5(3) . 5_556 O28 Mo2 O26 98.2(2) . . O28 Mo2 O22 170.4(2) . . O28 Mo2 O30 104.8(3) . . O28 Mo2 O29 94.4(2) . . Mo3 Mo4 Na2 87.59(2) . 10_554 Mo3 Mo4 Na2 87.59(2) . . Na2 Mo4 Na2 0.00(19) 10_554 . O23 Mo4 Mo3 49.03(15) . . O23 Mo4 Na2 129.10(15) . . O23 Mo4 Na2 129.10(15) . 10_554 O23 Mo4 O18 78.9(2) . . O23 Mo4 O10 157.6(2) . . O23 Mo4 O15 86.9(2) . . O18 Mo4 Mo3 87.79(13) . . O18 Mo4 Na2 73.52(16) . 10_554 O18 Mo4 Na2 73.52(16) . . O10 Mo4 Mo3 133.26(16) . . O10 Mo4 Na2 45.67(16) . . O10 Mo4 Na2 45.67(16) . 10_554 O10 Mo4 O18 78.98(19) . . O15 Mo4 Mo3 134.82(15) . . O15 Mo4 Na2 122.13(16) . 10_554 O15 Mo4 Na2 122.13(16) . . O15 Mo4 O18 71.91(19) . . O15 Mo4 O10 82.9(2) . . O17 Mo4 Mo3 48.17(16) . . O17 Mo4 Na2 40.21(16) . . O17 Mo4 Na2 40.21(16) . 10_554 O17 Mo4 O23 95.2(2) . . O17 Mo4 O18 82.9(2) . . O17 Mo4 O10 85.5(2) . . O17 Mo4 O15 153.8(2) . . O16 Mo4 Mo3 101.4(2) . . O16 Mo4 Na2 109.4(2) . 10_554 O16 Mo4 Na2 109.4(2) . . O16 Mo4 O23 104.9(3) . . O16 Mo4 O18 170.4(2) . . O16 Mo4 O10 96.5(2) . . O16 Mo4 O15 99.2(3) . . O16 Mo4 O17 105.4(3) . . O23 Mo3 Mo4 49.26(16) . . O23 Mo3 O26 86.2(2) . . O23 Mo3 O22 79.8(2) . . O23 Mo3 O27 159.4(2) . . O26 Mo3 Mo4 134.93(14) . . O26 Mo3 O22 72.41(19) . . O22 Mo3 Mo4 90.36(13) . . O17 Mo3 Mo4 47.93(16) . . O17 Mo3 O23 95.1(2) . . O17 Mo3 O26 157.2(2) . . O17 Mo3 O22 85.4(2) . . O17 Mo3 O27 86.1(2) . . O27 Mo3 Mo4 133.75(16) . . O27 Mo3 O26 84.9(2) . . O27 Mo3 O22 79.87(19) . . O24 Mo3 Mo4 101.2(2) . . O24 Mo3 O23 104.0(2) . . O24 Mo3 O26 95.6(3) . . O24 Mo3 O22 167.4(2) . . O24 Mo3 O17 106.1(3) . . O24 Mo3 O27 95.3(2) . . O19 Mo5 Mo6 40.92(15) . . O19 Mo5 O18 81.4(2) . . O19 Mo5 O11 156.0(2) . . O18 Mo5 Mo6 85.25(13) . . O15 Mo5 Mo6 134.37(17) . . O15 Mo5 O19 94.6(2) . . O15 Mo5 O18 76.2(2) . . O15 Mo5 O11 90.9(2) . . O15 Mo5 O13 158.6(2) . . O11 Mo5 Mo6 125.38(15) . . O11 Mo5 O18 77.4(2) . . O13 Mo5 Mo6 39.93(15) . . O13 Mo5 O19 80.1(2) . . O13 Mo5 O18 82.4(2) . . O13 Mo5 O11 86.2(2) . . O14 Mo5 Mo6 98.8(2) . . O14 Mo5 O19 102.3(3) . . O14 Mo5 O18 175.8(3) . . O14 Mo5 O15 101.3(3) . . O14 Mo5 O11 99.4(3) . . O14 Mo5 O13 100.1(3) . . O19 Mo6 Mo5 41.04(15) . . O19 Mo6 O21 81.6(2) . . O19 Mo6 O34 160.8(2) . . O21 Mo6 Mo5 83.40(12) . . O32 Mo6 Mo5 132.98(16) . . O32 Mo6 O19 94.2(2) . . O32 Mo6 O21 74.6(2) . . O32 Mo6 O13 153.9(2) . . O32 Mo6 O34 88.2(2) . . O13 Mo6 Mo5 40.87(16) . . O13 Mo6 O19 81.2(2) . . O13 Mo6 O21 79.3(2) . . O13 Mo6 O34 88.3(2) . . O34 Mo6 Mo5 128.82(16) . . O34 Mo6 O21 80.7(2) . . O20 Mo6 Mo5 99.8(2) . . O20 Mo6 O19 100.8(3) . . O20 Mo6 O21 176.8(3) . . O20 Mo6 O32 103.1(3) . . O20 Mo6 O13 103.0(3) . . O20 Mo6 O34 97.1(3) . . O25 Fe2 O25 82.2(3) . 5_556 O23 Fe2 O25 94.94(19) . 5_556 O23 Fe2 O25 94.94(19) 5_556 . O23 Fe2 O25 84.72(19) 5_556 5_556 O23 Fe2 O25 84.71(19) . . O23 Fe2 O23 179.5(3) . 5_556 O19 Fe2 O25 97.15(19) 5_556 . O19 Fe2 O25 179.3(2) . . O19 Fe2 O25 97.15(19) . 5_556 O19 Fe2 O25 179.3(2) 5_556 5_556 O19 Fe2 O23 85.09(19) 5_556 . O19 Fe2 O23 85.09(19) . 5_556 O19 Fe2 O23 95.25(19) 5_556 5_556 O19 Fe2 O23 95.25(19) . . O19 Fe2 O19 83.5(3) 5_556 . O2 Fe1 O12 88.4(2) . 27_566 O1 Fe1 O2 82.4(2) . . O1 Fe1 O3 88.8(2) . . O1 Fe1 O8 91.3(2) . . O1 Fe1 O12 92.4(2) . 27_566 O3 Fe1 O2 168.1(2) . . O3 Fe1 O8 101.5(2) . . O3 Fe1 O12 83.9(2) . 27_566 O8 Fe1 O2 86.8(2) . . O8 Fe1 O12 173.5(2) . 27_566 O4 Fe1 O2 90.3(2) . . O4 Fe1 O1 172.1(2) . . O4 Fe1 O3 97.9(2) . . O4 Fe1 O8 91.4(2) . . O4 Fe1 O12 84.3(2) . 27_566 O5 Fe3 O5 80.5(2) 17_666 . O5 Fe3 O1W 92.3(3) 17_666 . O5 Fe3 O6 82.4(3) . . O5 Fe3 O6 80.1(2) 17_666 . O7 Fe3 O5 94.1(2) . . O7 Fe3 O5 162.1(2) . 17_666 O7 Fe3 O9 108.2(2) . 27_566 O7 Fe3 O1W 90.2(3) . . O7 Fe3 O6 82.3(3) . . O9 Fe3 O5 89.4(2) 27_566 17_666 O9 Fe3 O5 95.3(2) 27_566 . O9 Fe3 O1W 93.3(3) 27_566 . O9 Fe3 O6 169.5(3) 27_566 . O1W Fe3 O5 168.7(3) . . O1W Fe3 O6 87.7(3) . . O1 P1 O1 108.50(19) . 20_657 O1 P1 O1 108.49(19) . 27_566 O1 P1 O1 111.4(4) . 10_554 O1 P1 O1 111.4(4) 27_566 20_657 O1 P1 O1 108.49(19) 10_554 20_657 O1 P1 O1 108.49(19) 27_566 10_554 O21 P4 O22 107.7(3) . . O18 P4 O22 108.5(3) . . O18 P4 O21 108.6(3) . . O3 P4 O22 110.4(3) 10_554 . O3 P4 O21 113.1(3) 10_554 . O3 P4 O18 108.4(3) 10_554 . O5 P2 O29 107.3(3) . 10_554 O27 P2 O5 107.5(3) 10_554 . O27 P2 O29 108.9(3) 10_554 10_554 O4 P2 O5 109.9(3) . . O4 P2 O29 110.3(3) . 10_554 O4 P2 O27 112.8(3) . 10_554 O2 P5 O33 109.4(3) 20_657 . O2 P5 O34 107.2(3) 20_657 . O2 P5 O9 111.5(4) 20_657 . O33 P5 O34 110.0(3) . . O9 P5 O33 110.0(3) . . O9 P5 O34 108.7(3) . . O10 P3 O11 110.3(3) . . O8 P3 O10 106.6(3) . . O8 P3 O11 108.8(3) . . O7 P3 O10 108.8(3) . . O7 P3 O8 113.4(3) . . O7 P3 O11 108.9(3) . . O2 Na1 O8 65.33(18) . . O2 Na1 O11 78.5(2) . . O1 Na1 O2 68.4(2) . . O1 Na1 O8 68.37(19) . . O1 Na1 O11 124.0(2) . . O1 Na1 O12 100.0(2) . . O1 Na1 O13 162.6(3) . . O11 Na1 O8 56.89(17) . . O12 Na1 O2 106.2(2) . . O12 Na1 O8 167.3(2) . . O12 Na1 O11 132.7(2) . . O13 Na1 O2 128.9(2) . . O13 Na1 O8 117.5(2) . . O13 Na1 O11 67.14(19) . . O13 Na1 O12 75.2(2) . . Mo4 Na2 Mo4 143.61(19) . 10_554 P3 Na2 Mo4 58.30(4) 10_554 10_554 P3 Na2 Mo4 129.27(5) 10_554 . Na2 Na2 Mo4 0(10) 10_554 . Na2 Na2 Mo4 0(7) 10_554 10_554 Na2 Na2 P3 0(10) 10_554 10_554 Na2 Na2 O10 0(10) 10_554 10_554 Na2 Na2 O10 0(10) 10_554 . Na2 Na2 O8 0(10) 10_554 . Na2 Na2 O8 0(10) 10_554 10_554 Na2 Na2 O17 0(10) 10_554 10_554 Na2 Na2 O17 0(10) 10_554 . Na2 Na2 O4W 0(10) 10_554 . O10 Na2 Mo4 33.70(12) 10_554 10_554 O10 Na2 Mo4 132.71(19) . 10_554 O10 Na2 Mo4 33.70(12) . . O10 Na2 Mo4 132.71(19) 10_554 . O10 Na2 P3 29.38(12) 10_554 10_554 O10 Na2 P3 162.97(14) . 10_554 O10 Na2 O10 151.5(4) 10_554 . O10 Na2 O4W 75.76(18) . . O10 Na2 O4W 75.76(18) 10_554 . O8 Na2 Mo4 81.13(12) . . O8 Na2 Mo4 121.49(13) . 10_554 O8 Na2 Mo4 121.49(13) 10_554 . O8 Na2 Mo4 81.13(12) 10_554 10_554 O8 Na2 P3 132.6(3) . 10_554 O8 Na2 P3 28.40(12) 10_554 10_554 O8 Na2 O10 146.1(2) 10_554 . O8 Na2 O10 57.30(16) . . O8 Na2 O10 57.30(16) 10_554 10_554 O8 Na2 O10 146.1(2) . 10_554 O8 Na2 O8 107.8(3) 10_554 . O8 Na2 O17 106.00(18) 10_554 10_554 O8 Na2 O17 106.00(18) . . O8 Na2 O17 98.45(17) 10_554 . O8 Na2 O17 98.45(17) . 10_554 O8 Na2 O4W 126.11(17) . . O8 Na2 O4W 126.11(17) 10_554 . O17 Na2 Mo4 130.4(2) . 10_554 O17 Na2 Mo4 130.4(2) 10_554 . O17 Na2 Mo4 29.33(12) . . O17 Na2 Mo4 29.34(12) 10_554 10_554 O17 Na2 P3 100.19(13) . 10_554 O17 Na2 P3 86.93(13) 10_554 10_554 O17 Na2 O10 106.3(2) 10_554 . O17 Na2 O10 106.3(2) . 10_554 O17 Na2 O10 62.81(17) 10_554 10_554 O17 Na2 O10 62.81(17) . . O17 Na2 O17 138.0(4) . 10_554 O17 Na2 O4W 68.99(18) 10_554 . O17 Na2 O4W 68.99(18) . . O4W Na2 Mo4 71.81(10) . 10_554 O4W Na2 Mo4 71.80(10) . . O4W Na2 P3 99.92(12) . 10_554 Mo1 O25 Fe2 133.8(3) 5_556 . Mo2 O25 Mo1 82.4(2) 5_556 5_556 Mo2 O25 Fe2 134.4(3) 5_556 . Mo4 O23 Fe2 135.5(3) . . Mo3 O23 Mo4 81.7(2) . . Mo3 O23 Fe2 135.4(3) . . Mo5 O19 Fe2 128.7(3) . . Mo6 O19 Mo5 98.0(2) . . Mo6 O19 Fe2 126.7(3) . . Mo2 O26 Mo3 112.1(2) . . Mo3 O22 Mo2 102.03(19) . . P4 O22 Mo2 127.5(3) . . P4 O22 Mo3 125.1(3) . . Mo1 O21 Mo6 91.55(18) . . P4 O21 Mo1 126.2(3) . . P4 O21 Mo6 129.6(3) . . Mo2 O30 Mo1 83.8(2) . . Fe3 O5 Fe3 99.5(2) 17_666 . P2 O5 Fe3 120.9(3) . . P2 O5 Fe3 136.5(3) . 17_666 Mo5 O18 Mo4 93.54(18) . . P4 O18 Mo4 125.6(3) . . P4 O18 Mo5 132.8(3) . . Fe1 O2 Na1 88.5(2) . . P5 O2 Fe1 135.6(3) 27_566 . P5 O2 Na1 135.9(3) 27_566 . P2 O29 Mo2 128.9(3) 10_554 . Fe1 O1 Na1 94.0(2) . . P1 O1 Fe1 144.9(3) . . P1 O1 Na1 118.3(3) . . Mo6 O32 Mo1 119.6(3) . . Mo4 O10 Na2 100.6(2) . 10_554 Mo4 O10 Na2 100.6(2) . . P3 O10 Mo4 135.6(3) . . P3 O10 Na2 91.7(3) . 10_554 P3 O10 Na2 91.7(3) . . Na2 O10 Na2 0.0(3) 10_554 . Mo5 O15 Mo4 117.9(3) . . P4 O3 Fe1 138.2(3) 10_554 . Fe1 O8 Na1 80.23(18) . . Fe1 O8 Na2 116.4(2) . . Fe1 O8 Na2 116.4(2) . 10_554 P3 O8 Fe1 132.6(3) . . P3 O8 Na1 94.3(3) . . P3 O8 Na2 102.8(3) . 10_554 P3 O8 Na2 102.8(3) . . Na2 O8 Na1 130.7(2) 10_554 . Na2 O8 Na1 130.7(2) . . Na2 O8 Na2 0.0(3) 10_554 . Mo5 O11 Na1 96.7(2) . . P3 O11 Mo5 134.1(3) . . P3 O11 Na1 99.9(3) . . Fe1 O12 Na1 115.0(2) 20_657 . Mo4 O17 Mo3 83.9(2) . . Mo4 O17 Na2 110.5(2) . 10_554 Mo4 O17 Na2 110.5(2) . . Mo3 O17 Na2 160.4(3) . 10_554 Mo3 O17 Na2 160.4(3) . . Na2 O17 Na2 0.0(3) 10_554 . Mo3 O27 Na3 118.3(4) . 10_554 P2 O27 Mo3 130.5(3) 10_554 . P2 O27 Na3 108.4(4) 10_554 10_554 Mo5 O13 Na1 105.2(2) . . Mo6 O13 Mo5 99.2(2) . . Mo6 O13 Na1 142.0(3) . . P2 O4 Fe1 167.0(4) . . P5 O33 Mo1 138.4(3) . . P5 O34 Mo6 134.6(3) . . Fe3 O7 Na3 96.9(5) . . P3 O7 Fe3 143.5(4) . . P3 O7 Na3 119.4(5) . . P5 O9 Fe3 141.4(4) . 20_657 Fe3 O6 Na3 94.1(4) . . Na2 O4W Na2 0.0 10_554 . O27 Na3 O7 87.6(4) 10_554 . O27 Na3 O3WA 170.3(14) 10_554 . O7 Na3 O3WA 93.2(10) . . O6 Na3 O27 111.0(7) . 10_554 O6 Na3 O7 69.7(4) . . O6 Na3 O3WA 78.2(12) . . O2W Na3 O27 81.9(5) . 10_554 O2W Na3 O7 158.4(9) . . O2W Na3 O6 96.5(6) . . O2W Na3 O3WA 100.4(11) . . O3W Na3 O27 145.0(18) . 10_554 O3W Na3 O7 99.1(12) . . O3W Na3 O6 103.5(16) . . O3W Na3 O2W 100.3(12) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Mo1 Mo2 2.6006(9) . Mo1 O25 1.979(5) 5_556 Mo1 O21 2.279(5) . Mo1 O30 1.949(5) . Mo1 O32 2.049(5) . Mo1 O33 2.061(5) . Mo1 O31 1.684(5) . Mo2 O25 1.970(5) 5_556 Mo2 O26 2.093(5) . Mo2 O22 2.247(5) . Mo2 O30 1.945(5) . Mo2 O29 2.072(5) . Mo2 O28 1.674(5) . Mo4 Mo3 2.5778(9) . Mo4 Na2 3.681(2) 10_554 Mo4 Na2 3.681(2) . Mo4 O23 1.974(5) . Mo4 O18 2.301(5) . Mo4 O10 2.078(5) . Mo4 O15 2.059(5) . Mo4 O17 1.924(5) . Mo4 O16 1.677(5) . Mo3 O23 1.967(5) . Mo3 O26 2.114(5) . Mo3 O22 2.242(5) . Mo3 O17 1.932(5) . Mo3 O27 2.071(5) . Mo3 O24 1.686(5) . Mo5 Mo6 2.9590(10) . Mo5 O19 1.962(5) . Mo5 O18 2.283(5) . Mo5 O15 1.837(5) . Mo5 O11 2.002(5) . Mo5 O13 1.961(5) . Mo5 O14 1.676(6) . Mo6 O19 1.957(5) . Mo6 O21 2.401(5) . Mo6 O32 1.829(5) . Mo6 O13 1.924(5) . Mo6 O34 2.023(5) . Mo6 O20 1.672(5) . Fe2 O25 2.189(5) 5_556 Fe2 O25 2.189(5) . Fe2 O23 2.181(5) . Fe2 O23 2.181(5) 5_556 Fe2 O19 2.168(5) 5_556 Fe2 O19 2.168(5) . Fe1 O2 2.029(5) . Fe1 O1 1.950(5) . Fe1 O3 1.966(5) . Fe1 O8 2.005(5) . Fe1 O12 2.150(5) 27_566 Fe1 O4 1.931(5) . Fe3 O5 2.129(5) . Fe3 O5 2.084(5) 17_666 Fe3 O7 1.980(6) . Fe3 O9 2.032(6) 27_566 Fe3 O1W 2.113(8) . Fe3 O6 2.243(8) . P1 O1 1.527(5) . P1 O1 1.527(5) 10_554 P1 O1 1.527(5) 20_657 P1 O1 1.527(5) 27_566 P4 O22 1.550(5) . P4 O21 1.542(5) . P4 O18 1.535(5) . P4 O3 1.520(5) 10_554 P2 O5 1.544(5) . P2 O29 1.549(5) 10_554 P2 O27 1.534(5) 10_554 P2 O4 1.488(5) . P5 O2 1.499(5) 20_657 P5 O33 1.533(5) . P5 O34 1.562(6) . P5 O9 1.527(6) . P3 O10 1.534(6) . P3 O8 1.524(5) . P3 O11 1.568(5) . P3 O7 1.511(6) . Na1 O2 2.390(6) . Na1 O1 2.270(6) . Na1 O8 2.720(6) . Na1 O11 2.551(6) . Na1 O12 2.354(6) . Na1 O13 2.336(6) . Na2 Na2 0.000(13) 10_554 Na2 O10 2.679(6) 10_554 Na2 O10 2.679(6) . Na2 O8 2.412(6) . Na2 O8 2.412(6) 10_554 Na2 O17 2.536(6) 10_554 Na2 O17 2.536(6) . Na2 O4W 2.78(5) . O27 Na3 2.487(13) 10_554 O7 Na3 2.504(11) . O6 Na3 2.368(18) . O2W Na3 2.344(16) . Na3 O3W 1.84(4) . Na3 O3WA 2.62(6) . 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_4 Mo5 Mo6 O32 Mo1 71.6(3) . . Mo6 Mo5 O15 Mo4 -74.5(3) . . O19 Mo5 O15 Mo4 -85.5(3) . . O19 Mo6 O32 Mo1 86.6(3) . . O22 P4 O21 Mo1 10.9(4) . . O22 P4 O21 Mo6 -119.6(4) . . O22 P4 O18 Mo4 -17.0(4) . . O22 P4 O18 Mo5 123.2(4) . . O21 Mo6 O32 Mo1 6.5(2) . . O21 P4 O22 Mo2 -13.8(4) . . O21 P4 O22 Mo3 135.6(3) . . O21 P4 O18 Mo4 -133.8(3) . . O21 P4 O18 Mo5 6.4(5) . . O5 P2 O4 Fe1 150.1(16) . . O18 Mo5 O15 Mo4 -5.5(3) . . O18 P4 O22 Mo2 -131.2(3) . . O18 P4 O22 Mo3 18.2(4) . . O18 P4 O21 Mo1 128.2(3) . . O18 P4 O21 Mo6 -2.2(5) . . O2 P5 O33 Mo1 -112.2(5) 20_657 . O2 P5 O34 Mo6 116.0(5) 20_657 . O2 P5 O9 Fe3 -4.7(7) 20_657 20_657 O29 P2 O5 Fe3 -146.8(3) 10_554 . O29 P2 O5 Fe3 9.1(6) 10_554 17_666 O29 P2 O4 Fe1 -91.9(17) 10_554 . O1 P1 O1 Fe1 -62.2(5) 10_554 . O1 P1 O1 Fe1 57.2(4) 27_566 . O1 P1 O1 Fe1 178.4(6) 20_657 . O1 P1 O1 Na1 92.1(3) 10_554 . O1 P1 O1 Na1 -148.5(4) 27_566 . O1 P1 O1 Na1 -27.2(2) 20_657 . O10 P3 O8 Fe1 158.4(4) . . O10 P3 O8 Na1 -120.9(3) . . O10 P3 O8 Na2 12.6(3) . . O10 P3 O8 Na2 12.6(3) . 10_554 O10 P3 O11 Mo5 9.2(5) . . O10 P3 O11 Na1 118.7(3) . . O10 P3 O7 Fe3 154.5(5) . . O10 P3 O7 Na3 -31.0(5) . . O3 P4 O22 Mo2 110.1(4) 10_554 . O3 P4 O22 Mo3 -100.5(4) 10_554 . O3 P4 O21 Mo1 -111.4(4) 10_554 . O3 P4 O21 Mo6 118.1(4) 10_554 . O3 P4 O18 Mo4 103.0(4) 10_554 . O3 P4 O18 Mo5 -116.8(4) 10_554 . O8 P3 O10 Mo4 96.0(5) . . O8 P3 O10 Na2 -11.0(3) . . O8 P3 O10 Na2 -11.0(3) . 10_554 O8 P3 O11 Mo5 -107.4(4) . . O8 P3 O11 Na1 2.1(3) . . O8 P3 O7 Fe3 -87.1(6) . . O8 P3 O7 Na3 87.4(5) . . O11 Mo5 O15 Mo4 71.2(3) . . O11 P3 O10 Mo4 -22.0(6) . . O11 P3 O10 Na2 -129.0(3) . . O11 P3 O10 Na2 -129.0(3) . 10_554 O11 P3 O8 Fe1 -82.6(5) . . O11 P3 O8 Na1 -1.9(3) . . O11 P3 O8 Na2 131.5(3) . 10_554 O11 P3 O8 Na2 131.5(3) . . O11 P3 O7 Fe3 34.3(7) . . O11 P3 O7 Na3 -151.3(4) . . O27 P2 O5 Fe3 96.2(4) 10_554 . O27 P2 O5 Fe3 -107.9(5) 10_554 17_666 O27 P2 O4 Fe1 30.2(18) 10_554 . O13 Mo5 O15 Mo4 -10.8(8) . . O13 Mo6 O32 Mo1 8.2(7) . . O4 P2 O5 Fe3 129.1(5) . 17_666 O4 P2 O5 Fe3 -26.8(4) . . O33 P5 O34 Mo6 -2.9(6) . . O33 P5 O9 Fe3 116.8(6) . 20_657 O34 Mo6 O32 Mo1 -74.3(3) . . O34 P5 O33 Mo1 5.4(6) . . O34 P5 O9 Fe3 -122.7(6) . 20_657 O7 P3 O10 Mo4 -141.4(4) . . O7 P3 O10 Na2 111.5(3) . . O7 P3 O10 Na2 111.5(3) . 10_554 O7 P3 O8 Fe1 38.8(5) . . O7 P3 O8 Na1 119.5(3) . . O7 P3 O8 Na2 -107.0(3) . 10_554 O7 P3 O8 Na2 -107.0(3) . . O7 P3 O11 Mo5 128.5(4) . . O7 P3 O11 Na1 -122.0(3) . . O20 Mo6 O32 Mo1 -171.3(3) . . O9 P5 O33 Mo1 125.0(5) . . O9 P5 O34 Mo6 -123.4(5) . . O14 Mo5 O15 Mo4 170.9(3) . .