#------------------------------------------------------------------------------ #$Date: 2020-02-04 22:10:48 +0200 (Tue, 04 Feb 2020) $ #$Revision: 247622 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/56/7125641.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_7125641 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 O1156 P136), 54(O)' _chemical_formula_sum 'Fe40 Mo96 Na32 O632 P68' _chemical_formula_weight 24397.88 _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 2019-03-27 _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 27.3329(12) _cell_length_b 27.3329(12) _cell_length_c 37.8621(14) _cell_measurement_reflns_used 9885 _cell_measurement_temperature 100 _cell_measurement_theta_max 26.01 _cell_measurement_theta_min 2.59 _cell_volume 28286(2) _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 0.995 _diffrn_measured_fraction_theta_max 0.992 _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 0.0398 _diffrn_reflns_av_unetI/netI 0.0207 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_number 73586 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.065 _diffrn_reflns_theta_min 2.590 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.392 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 2.865 _exptl_crystal_description block _exptl_crystal_F_000 23000 _refine_diff_density_max 1.360 _refine_diff_density_min -1.044 _refine_diff_density_rms 0.170 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 546 _refine_ls_number_reflns 6960 _refine_ls_number_restraints 72 _refine_ls_restrained_S_all 1.058 _refine_ls_R_factor_all 0.0420 _refine_ls_R_factor_gt 0.0317 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+461.1291P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0897 _refine_ls_wR_factor_ref 0.0962 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5905 _reflns_number_total 6960 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc08696j2.cif _cod_data_source_block 2 _cod_depositor_comments 'Adding full bibliography for 7125640--7125641.cif.' _cod_original_cell_volume 28286(3) _cod_original_sg_symbol_H-M 'I 41/a c d' _cod_database_code 7125641 _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(O10W) \\sim Ueq, Uanis(O12W) \\sim Ueq, Uanis(O9W) \\sim Ueq, Uanis(O8W) \\sim Ueq, Uanis(O5W) \\sim Ueq, Uanis(O11W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O4W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O7W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O3WA) \\sim Ueq, Uanis(O3W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O6W) \\sim Ueq, Uanis(O13W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 2. Others Fixed Sof: O3W(0.5) O8W(0.5) O9W(0.5) O11W(0.5) O12W(0.25) O5W(0.5) O10W(0.5) O4W(0.125) O3WA(0.5) O7W(0.125) O13W(0.25) O6W(0.25) ; _shelx_res_file ; TITL w_a.res in I4(1)/acd 2.res created by SHELXL-2017/1 at 20:42:41 on 27-Mar-2019 REM Old TITL w in I4(1)/acd REM SHELXT solution in I4(1)/acd REM R1 0.152, Rweak 0.002, Alpha 0.017, Orientation as input REM Formula found by SHELXT: O148 P16 S Mo24 Fe10 CELL 0.71073 27.3329 27.3329 37.8621 90 90 90 ZERR 2 0.0012 0.0012 0.0014 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 1264 136 EQIV $1 1-X,1.5-Y,+Z EQIV $2 -0.25+Y,1.25-X,0.75-Z EQIV $3 1.25-Y,0.25+X,0.75-Z ISOR 0.01 0.02 O10W O12W O9W O8W O5W O11W ISOR 0.01 0.02 O4W ISOR 0.01 0.02 O7W ISOR 0.01 0.02 O3WA O3W ISOR 0.01 0.02 O6W O13W L.S. 4 PLAN 20 TEMP -173.15 FREE P3 Na1 FREE P2 Na1 FREE P2 Na2_$1 FREE P2 Na2 FREE Mo1 Na2_$1 FREE Mo1 Na2 FREE Fe1 Na1 FREE Mo6 Na1 FREE P1 Na1_$1 FREE P1 Na1_$3 FREE P1 Na1_$2 FREE P1 Na1 list 4 conf fmap 2.0 acta OMIT 2 2 4 OMIT 1 4 1 OMIT 0 2 4 OMIT 1 2 5 OMIT 0 6 0 OMIT 1 1 6 REM REM REM WGHT 0.049000 461.129089 FVAR 0.01866 MO3 2 0.319725 0.596801 0.466973 11.00000 0.00886 0.01109 = 0.01750 0.00209 0.00064 0.00008 MO2 2 0.371895 0.662299 0.536493 11.00000 0.01328 0.01384 = 0.01409 0.00041 0.00175 0.00251 MO4 2 0.282583 0.644056 0.413769 11.00000 0.01066 0.01296 = 0.01524 0.00227 0.00045 -0.00101 MO1 2 0.372069 0.756534 0.536688 11.00000 0.01277 0.01455 = 0.01492 -0.00149 0.00277 0.00031 MO6 2 0.319120 0.820288 0.471722 11.00000 0.01058 0.01327 = 0.02684 0.00047 0.00370 0.00106 MO5 2 0.272172 0.766581 0.412956 11.00000 0.01288 0.01764 = 0.01844 0.00290 0.00188 0.00322 FE1 1 0.518579 0.838859 0.432355 11.00000 0.00761 0.01087 = 0.01267 -0.00145 -0.00082 0.00038 FE2 1 0.250000 0.709591 0.500000 10.50000 0.01113 0.01348 = 0.01728 0.00000 0.00102 0.00000 FE3 1 0.289119 0.706720 0.255296 11.00000 0.01509 0.02129 = 0.02008 0.00106 -0.00311 -0.00133 P3 5 0.375559 0.707317 0.453415 11.00000 0.00797 0.00939 = 0.01377 0.00079 0.00105 0.00083 P1 5 0.500000 0.750000 0.375000 10.25000 0.01176 0.01176 = 0.00905 0.00000 0.00000 0.00000 P4 5 0.433541 0.580505 0.491376 11.00000 0.00809 0.00927 = 0.01603 0.00326 0.00096 0.00217 P5 5 0.312845 0.709423 0.341704 11.00000 0.01319 0.01430 = 0.01175 0.00210 -0.00123 -0.00224 P2 5 0.434251 0.841934 0.492017 11.00000 0.01159 0.01203 = 0.01687 -0.00307 0.00172 -0.00192 NA1 3 0.411935 0.813540 0.411722 11.00000 0.01870 0.05862 = 0.03484 -0.01449 0.00294 -0.00503 NA2 3 0.500000 0.750000 0.508411 10.50000 0.02837 0.02691 = 0.08256 0.00000 0.00000 0.00524 O22 4 0.270386 0.649173 0.465010 11.00000 0.01067 0.01799 = 0.01526 0.00462 0.00262 0.00205 O15 4 0.318827 0.709364 0.529033 11.00000 0.01242 0.01496 = 0.01858 0.00159 0.00472 0.00192 O18 4 0.270184 0.768793 0.464602 11.00000 0.01103 0.01858 = 0.01828 -0.00048 0.00191 -0.00295 O23 4 0.320674 0.607909 0.521586 11.00000 0.01419 0.01460 = 0.01822 0.00253 0.00246 -0.00073 O16 4 0.368110 0.661821 0.477371 11.00000 0.00946 0.01067 = 0.01605 0.00081 0.00120 -0.00049 O17 4 0.335151 0.706888 0.425100 11.00000 0.01276 0.01145 = 0.01675 0.00000 -0.00142 0.00009 O12 4 0.369604 0.753876 0.476096 11.00000 0.01257 0.01385 = 0.01688 -0.00139 0.00068 0.00080 O26 4 0.384429 0.560181 0.477190 11.00000 0.01059 0.01243 = 0.02756 0.00172 -0.00201 0.00236 O13 4 0.324300 0.810139 0.519353 11.00000 0.01473 0.01453 = 0.02165 -0.00172 0.00467 0.00139 O21 4 0.241858 0.706812 0.410417 11.00000 0.01268 0.01732 = 0.01920 0.00332 0.00035 -0.00141 O28 4 0.466516 0.536278 0.500896 11.00000 0.00986 0.01012 = 0.02445 0.00038 -0.00220 0.00347 O24 4 0.342169 0.605252 0.418487 11.00000 0.01474 0.01440 = 0.01621 -0.00195 0.00091 0.00136 O4 4 0.471575 0.815243 0.469127 11.00000 0.01434 0.01238 = 0.02000 -0.00165 0.00425 -0.00052 O29 4 0.424249 0.609442 0.525346 11.00000 0.01748 0.01825 = 0.01924 -0.00149 -0.00391 0.00759 O8 4 0.386525 0.850234 0.470134 11.00000 0.01212 0.01894 = 0.02147 0.00334 -0.00098 -0.00254 O9 4 0.327694 0.808618 0.421059 11.00000 0.01827 0.01555 = 0.01916 -0.00081 -0.00025 -0.00169 O11 4 0.426811 0.707384 0.438022 11.00000 0.01211 0.01527 = 0.02329 0.00254 0.00668 0.00118 O3 4 0.490122 0.795187 0.397634 11.00000 0.01122 0.02270 = 0.01686 -0.01151 -0.00167 0.00216 O5 4 0.575633 0.790586 0.530184 11.00000 0.01333 0.01959 = 0.02128 0.00497 -0.00127 0.00324 O7 4 0.424145 0.809248 0.524156 11.00000 0.02052 0.02190 = 0.01686 -0.00041 0.00153 -0.00372 O34 4 0.452322 0.891045 0.505116 11.00000 0.01955 0.01453 = 0.02919 -0.00660 0.00003 -0.00293 O2 4 0.464395 0.883174 0.415521 11.00000 0.01359 0.01680 = 0.02351 0.00364 -0.00281 0.00275 O19 4 0.297002 0.755721 0.363326 11.00000 0.01855 0.01571 = 0.01934 0.00088 0.00493 0.00217 O27 4 0.458260 0.610313 0.463208 11.00000 0.01370 0.01714 = 0.03001 0.00822 0.00688 -0.00020 O1 4 0.565932 0.872986 0.394451 11.00000 0.01920 0.02534 = 0.02324 0.00999 0.00031 -0.00230 O31 4 0.302974 0.662450 0.362978 11.00000 0.02535 0.01548 = 0.01652 0.00184 0.00280 -0.00565 O32 4 0.282871 0.708665 0.307642 11.00000 0.03056 0.02864 = 0.02218 0.00330 -0.01274 -0.00566 O25 4 0.285239 0.545833 0.466172 11.00000 0.01967 0.02033 = 0.03097 0.00452 -0.00043 -0.00423 O20 4 0.227755 0.806156 0.402833 11.00000 0.02002 0.02426 = 0.03229 0.00652 0.00083 0.00545 O33 4 0.353919 0.510953 0.651949 11.00000 0.02203 0.01668 = 0.02332 0.00130 0.00338 0.00362 O10 4 0.284923 0.871359 0.470420 11.00000 0.02374 0.02114 = 0.03700 0.00180 0.00406 0.00591 O30 4 0.368738 0.650383 0.580151 11.00000 0.03085 0.02536 = 0.01853 0.00126 0.00180 0.00277 O14 4 0.370769 0.768380 0.580059 11.00000 0.02691 0.02883 = 0.01634 -0.00119 0.00550 0.00065 NA3 3 0.341223 0.591223 0.625000 10.50000 0.07820 0.07820 = 0.07366 0.02851 -0.02851 -0.00962 O1W 4 0.282665 0.706801 0.197389 11.00000 0.03487 0.05781 = 0.03523 0.00762 -0.00378 0.00599 O2W 4 0.282818 0.630369 0.252523 11.00000 0.03155 0.03825 = 0.06642 -0.00769 -0.00242 -0.00433 PART 1 O3W 4 0.275307 0.589818 0.681531 10.50000 0.12825 0.11887 = 0.08667 -0.01873 -0.03372 0.03842 PART 0 O8W 4 0.551796 0.924035 0.600419 10.50000 0.10861 0.05632 = 0.03376 -0.02495 -0.00041 0.05152 O9W 4 0.497547 0.884874 0.562752 10.50000 0.05355 0.10029 = 0.01854 -0.02178 -0.01332 0.03245 O11W 4 0.329341 0.909977 0.549267 10.50000 0.11148 0.06138 = 0.08937 -0.05015 0.03186 -0.04933 O12W 4 0.250000 0.961719 0.500000 10.25000 0.12961 0.06061 = 0.12238 0.00000 -0.02437 0.00000 O5W 4 0.373364 0.500257 0.407356 10.50000 0.12471 0.08644 = 0.10547 -0.02691 0.04495 0.01668 O10W 4 0.434943 0.877545 0.593334 10.50000 0.17469 0.11463 = 0.13042 0.02981 -0.09212 -0.06064 O4W 4 0.500000 0.750000 0.578020 10.12500 0.04292 0.07755 = 0.04170 0.00000 0.00000 -0.00959 PART 2 O3WA 4 0.291680 0.615948 0.672071 10.50000 0.07576 0.15649 = 0.06933 -0.02797 -0.03866 0.02084 PART 0 O7W 4 0.449757 0.699757 0.625000 10.12500 0.09931 0.09931 = 0.09303 0.05330 -0.05330 -0.02443 O13W 4 0.334222 0.536442 0.356709 10.25000 0.13431 0.14727 = 0.11643 -0.06351 0.04460 0.01069 O6W 4 0.247987 0.469632 0.430124 10.25000 0.10836 0.10233 = 0.15393 -0.04044 -0.00523 -0.01700 HKLF 4 REM w_a.res in I4(1)/acd REM R1 = 0.0317 for 5905 Fo > 4sig(Fo) and 0.0420 for all 6960 data REM 546 parameters refined using 72 restraints END WGHT 0.0490 461.0799 REM Highest difference peak 1.360, deepest hole -1.044, 1-sigma level 0.170 Q1 1 0.2017 0.5845 0.6828 11.00000 0.05 1.36 Q2 1 0.3185 0.8187 0.4495 11.00000 0.05 1.24 Q3 1 0.4989 0.7842 0.5842 11.00000 0.05 1.15 Q4 1 0.4824 0.6877 0.5995 11.00000 0.05 1.14 Q5 1 0.5383 0.9040 0.6023 11.00000 0.05 1.04 Q6 1 0.5796 0.9329 0.5944 11.00000 0.05 1.01 Q7 1 0.3113 0.9302 0.5332 11.00000 0.05 0.94 Q8 1 0.5510 0.9281 0.6104 11.00000 0.05 0.84 Q9 1 0.4656 0.8784 0.5718 11.00000 0.05 0.83 Q10 1 0.4561 0.8464 0.5975 11.00000 0.05 0.79 Q11 1 0.4104 0.8900 0.6030 11.00000 0.05 0.75 Q12 1 0.3182 0.9069 0.5661 11.00000 0.05 0.75 Q13 1 0.3175 0.6053 0.4877 11.00000 0.05 0.74 Q14 1 0.5926 0.8802 0.4031 11.00000 0.05 0.72 Q15 1 0.3387 0.5079 0.3861 11.00000 0.05 0.72 Q16 1 0.4061 0.8900 0.6354 11.00000 0.05 0.71 Q17 1 0.5143 0.8589 0.4256 11.00000 0.05 0.69 Q18 1 0.2978 0.7633 0.3935 11.00000 0.05 0.68 Q19 1 0.5554 0.8991 0.3859 11.00000 0.05 0.66 Q20 1 0.3227 0.5638 0.3408 11.00000 0.05 0.66 ; _shelx_res_checksum 3312 _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 Mo3 Mo 0.31973(2) 0.59680(2) 0.46697(2) 0.01249(11) Uani 1 1 d . . . . . Mo2 Mo 0.37190(2) 0.66230(2) 0.53649(2) 0.01373(12) Uani 1 1 d . . . . . Mo4 Mo 0.28258(2) 0.64406(2) 0.41377(2) 0.01295(11) Uani 1 1 d . . . . . Mo1 Mo 0.37207(2) 0.75653(2) 0.53669(2) 0.01408(12) Uani 1 1 d . . . . . Mo6 Mo 0.31912(2) 0.82029(2) 0.47172(2) 0.01690(12) Uani 1 1 d . . . . . Mo5 Mo 0.27217(2) 0.76658(2) 0.41296(2) 0.01632(12) Uani 1 1 d . . . . . Fe1 Fe 0.51858(3) 0.83886(3) 0.43235(2) 0.01038(16) Uani 1 1 d . . . . . Fe2 Fe 0.250000 0.70959(4) 0.500000 0.0140(2) Uani 1 2 d S T P . . Fe3 Fe 0.28912(3) 0.70672(3) 0.25530(2) 0.01882(19) Uani 1 1 d . . . . . P3 P 0.37556(5) 0.70732(5) 0.45342(4) 0.0104(3) Uani 1 1 d . . . . . P1 P 0.500000 0.750000 0.375000 0.0109(5) Uani 1 4 d S T P . . P4 P 0.43354(5) 0.58050(5) 0.49138(4) 0.0111(3) Uani 1 1 d . . . . . P5 P 0.31285(5) 0.70942(5) 0.34170(4) 0.0131(3) Uani 1 1 d . . . . . P2 P 0.43425(5) 0.84193(5) 0.49202(4) 0.0135(3) Uani 1 1 d . . . . . Na1 Na 0.41194(10) 0.81354(12) 0.41172(7) 0.0374(7) Uani 1 1 d . . . . . Na2 Na 0.500000 0.750000 0.50841(14) 0.0459(11) Uani 1 2 d S T P . . O22 O 0.27039(13) 0.64917(14) 0.46501(10) 0.0146(8) Uani 1 1 d . . . . . O15 O 0.31883(14) 0.70936(14) 0.52903(10) 0.0153(8) Uani 1 1 d . . . . . O18 O 0.27018(14) 0.76879(14) 0.46460(10) 0.0160(8) Uani 1 1 d . . . . . O23 O 0.32067(14) 0.60791(14) 0.52159(10) 0.0157(8) Uani 1 1 d . . . . . O16 O 0.36811(13) 0.66182(13) 0.47737(10) 0.0121(8) Uani 1 1 d . . . . . O17 O 0.33515(14) 0.70689(13) 0.42510(10) 0.0137(8) Uani 1 1 d . . . . . O12 O 0.36960(13) 0.75388(14) 0.47610(10) 0.0144(8) Uani 1 1 d . . . . . O26 O 0.38443(14) 0.56018(14) 0.47719(11) 0.0169(8) Uani 1 1 d . . . . . O13 O 0.32430(14) 0.81014(14) 0.51935(10) 0.0170(8) Uani 1 1 d . . . . . O21 O 0.24186(14) 0.70681(14) 0.41042(10) 0.0164(8) Uani 1 1 d . . . . . O28 O 0.46652(13) 0.53628(13) 0.50090(10) 0.0148(8) Uani 1 1 d . . . . . O24 O 0.34217(14) 0.60525(14) 0.41849(10) 0.0151(8) Uani 1 1 d . . . . . O4 O 0.47157(14) 0.81524(14) 0.46913(10) 0.0156(8) Uani 1 1 d . . . . . O29 O 0.42425(14) 0.60944(14) 0.52535(10) 0.0183(8) Uani 1 1 d . . . . . O8 O 0.38652(14) 0.85023(14) 0.47013(10) 0.0175(8) Uani 1 1 d . . . . . O9 O 0.32769(14) 0.80862(14) 0.42106(10) 0.0177(8) Uani 1 1 d . . . . . O11 O 0.42681(14) 0.70738(14) 0.43802(10) 0.0169(8) Uani 1 1 d . . . . . O3 O 0.49012(14) 0.79519(14) 0.39763(10) 0.0169(8) Uani 1 1 d . . . . . O5 O 0.57563(14) 0.79059(14) 0.53018(10) 0.0181(9) Uani 1 1 d . . . . . O7 O 0.42415(15) 0.80925(15) 0.52416(10) 0.0198(9) Uani 1 1 d . . . . . O34 O 0.45232(15) 0.89105(15) 0.50512(11) 0.0211(9) Uani 1 1 d . . . . . O2 O 0.46439(14) 0.88317(14) 0.41552(11) 0.0180(8) Uani 1 1 d . . . . . O19 O 0.29700(14) 0.75572(14) 0.36333(10) 0.0179(8) Uani 1 1 d . . . . . O27 O 0.45826(14) 0.61031(15) 0.46321(11) 0.0203(9) Uani 1 1 d . . . . . O1 O 0.56593(15) 0.87299(16) 0.39445(11) 0.0226(9) Uani 1 1 d . . . . . O31 O 0.30297(15) 0.66245(14) 0.36298(10) 0.0191(9) Uani 1 1 d . . . . . O32 O 0.28287(17) 0.70867(16) 0.30764(12) 0.0271(10) Uani 1 1 d . . . . . O25 O 0.28524(15) 0.54583(16) 0.46617(11) 0.0237(9) Uani 1 1 d . . . . . O20 O 0.22775(16) 0.80616(16) 0.40283(12) 0.0255(10) Uani 1 1 d . . . . . O33 O 0.35392(15) 0.51095(15) 0.65195(11) 0.0207(9) Uani 1 1 d . . . . . O10 O 0.28492(16) 0.87136(16) 0.47042(12) 0.0273(10) Uani 1 1 d . . . . . O30 O 0.36874(16) 0.65038(16) 0.58015(11) 0.0249(10) Uani 1 1 d . . . . . O14 O 0.37077(16) 0.76838(16) 0.58006(11) 0.0240(9) Uani 1 1 d . . . . . Na3 Na 0.34122(16) 0.59122(16) 0.625000 0.0767(18) Uani 1 2 d S T P . . O1W O 0.28267(19) 0.7068(2) 0.19739(14) 0.0426(13) Uani 1 1 d . . . . . O2W O 0.28282(19) 0.6304(2) 0.25252(16) 0.0454(14) Uani 1 1 d . . . . . O3W O 0.2753(10) 0.5898(9) 0.6815(7) 0.111(8) Uani 0.5 1 d . U . A 1 O8W O 0.5518(6) 0.9240(5) 0.6004(3) 0.066(4) Uani 0.5 1 d . U . . . O9W O 0.4975(4) 0.8849(5) 0.5628(3) 0.057(3) Uani 0.5 1 d . U . . . O11W O 0.3293(6) 0.9100(5) 0.5493(4) 0.087(5) Uani 0.5 1 d . U . . . O12W O 0.250000 0.9617(8) 0.500000 0.104(8) Uani 0.5 2 d S TU P . . O5W O 0.3734(7) 0.5003(7) 0.4074(5) 0.106(6) Uani 0.5 1 d . U . . . O10W O 0.4349(9) 0.8775(8) 0.5933(6) 0.140(8) Uani 0.5 1 d . U . . . O4W O 0.500000 0.750000 0.5780(8) 0.054(8) Uani 0.25 2 d S TU P . . O3WA O 0.2917(8) 0.6159(10) 0.6721(6) 0.101(7) Uani 0.5 1 d . U . A 2 O7W O 0.4498(12) 0.6998(12) 0.625000 0.097(13) Uani 0.25 2 d S TU P . . O13W O 0.3342(17) 0.5364(17) 0.3567(11) 0.133(14) Uani 0.25 1 d . U . . . O6W O 0.2480(16) 0.4696(15) 0.4301(12) 0.122(13) Uani 0.25 1 d . U . . . 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 Mo3 0.0089(2) 0.0111(2) 0.0175(2) 0.00209(17) 0.00064(17) 0.00008(17) Mo2 0.0133(2) 0.0138(2) 0.0141(2) 0.00041(18) 0.00175(18) 0.00251(18) Mo4 0.0107(2) 0.0130(2) 0.0152(2) 0.00227(18) 0.00045(17) -0.00101(18) Mo1 0.0128(2) 0.0146(2) 0.0149(2) -0.00149(18) 0.00277(18) 0.00031(18) Mo6 0.0106(2) 0.0133(2) 0.0268(3) 0.0005(2) 0.00370(19) 0.00106(19) Mo5 0.0129(2) 0.0176(3) 0.0184(3) 0.00290(19) 0.00188(18) 0.00322(19) Fe1 0.0076(3) 0.0109(4) 0.0127(4) -0.0015(3) -0.0008(3) 0.0004(3) Fe2 0.0111(5) 0.0135(5) 0.0173(6) 0.000 0.0010(4) 0.000 Fe3 0.0151(4) 0.0213(4) 0.0201(4) 0.0011(3) -0.0031(3) -0.0013(3) P3 0.0080(6) 0.0094(6) 0.0138(7) 0.0008(5) 0.0011(5) 0.0008(5) P1 0.0118(8) 0.0118(8) 0.0091(13) 0.000 0.000 0.000 P4 0.0081(6) 0.0093(6) 0.0160(7) 0.0033(5) 0.0010(5) 0.0022(5) P5 0.0132(7) 0.0143(7) 0.0118(7) 0.0021(5) -0.0012(5) -0.0022(5) P2 0.0116(7) 0.0120(7) 0.0169(7) -0.0031(5) 0.0017(5) -0.0019(5) Na1 0.0187(13) 0.0586(19) 0.0348(16) -0.0145(14) 0.0029(11) -0.0050(13) Na2 0.028(2) 0.027(2) 0.083(3) 0.000 0.000 0.0052(18) O22 0.0107(18) 0.018(2) 0.0153(19) 0.0046(15) 0.0026(15) 0.0020(16) O15 0.0124(19) 0.015(2) 0.019(2) 0.0016(15) 0.0047(15) 0.0019(15) O18 0.0110(19) 0.019(2) 0.018(2) -0.0005(16) 0.0019(15) -0.0030(16) O23 0.0142(19) 0.0146(19) 0.018(2) 0.0025(15) 0.0025(15) -0.0007(16) O16 0.0095(18) 0.0107(18) 0.0160(19) 0.0008(14) 0.0012(14) -0.0005(14) O17 0.0128(19) 0.0114(19) 0.017(2) 0.0000(15) -0.0014(15) 0.0001(15) O12 0.0126(19) 0.0139(19) 0.017(2) -0.0014(15) 0.0007(15) 0.0008(15) O26 0.0106(19) 0.0124(19) 0.028(2) 0.0017(16) -0.0020(16) 0.0024(15) O13 0.015(2) 0.0145(19) 0.022(2) -0.0017(16) 0.0047(16) 0.0014(16) O21 0.0127(19) 0.017(2) 0.019(2) 0.0033(16) 0.0003(15) -0.0014(16) O28 0.0099(18) 0.0101(18) 0.024(2) 0.0004(16) -0.0022(15) 0.0035(15) O24 0.0147(19) 0.0144(19) 0.0162(19) -0.0019(15) 0.0009(15) 0.0014(16) O4 0.0143(19) 0.0124(19) 0.020(2) -0.0017(15) 0.0043(16) -0.0005(16) O29 0.017(2) 0.018(2) 0.019(2) -0.0015(16) -0.0039(16) 0.0076(17) O8 0.0121(19) 0.019(2) 0.021(2) 0.0033(16) -0.0010(16) -0.0025(16) O9 0.018(2) 0.016(2) 0.019(2) -0.0008(16) -0.0003(16) -0.0017(16) O11 0.0121(19) 0.015(2) 0.023(2) 0.0025(16) 0.0067(16) 0.0012(15) O3 0.0112(19) 0.023(2) 0.017(2) -0.0115(16) -0.0017(15) 0.0022(16) O5 0.0133(19) 0.020(2) 0.021(2) 0.0050(16) -0.0013(16) 0.0032(16) O7 0.021(2) 0.022(2) 0.017(2) -0.0004(16) 0.0015(16) -0.0037(18) O34 0.020(2) 0.015(2) 0.029(2) -0.0066(17) 0.0000(17) -0.0029(17) O2 0.0136(19) 0.017(2) 0.024(2) 0.0036(16) -0.0028(16) 0.0028(16) O19 0.019(2) 0.016(2) 0.019(2) 0.0009(16) 0.0049(16) 0.0022(16) O27 0.014(2) 0.017(2) 0.030(2) 0.0082(17) 0.0069(17) -0.0002(16) O1 0.019(2) 0.025(2) 0.023(2) 0.0100(18) 0.0003(17) -0.0023(18) O31 0.025(2) 0.015(2) 0.017(2) 0.0018(16) 0.0028(17) -0.0057(17) O32 0.031(2) 0.029(2) 0.022(2) 0.0033(18) -0.0127(19) -0.006(2) O25 0.020(2) 0.020(2) 0.031(2) 0.0045(18) -0.0004(18) -0.0042(18) O20 0.020(2) 0.024(2) 0.032(2) 0.0065(19) 0.0008(18) 0.0055(18) O33 0.022(2) 0.017(2) 0.023(2) 0.0013(17) 0.0034(17) 0.0036(17) O10 0.024(2) 0.021(2) 0.037(3) 0.0018(19) 0.0041(19) 0.0059(19) O30 0.031(2) 0.025(2) 0.019(2) 0.0013(18) 0.0018(18) 0.0028(19) O14 0.027(2) 0.029(2) 0.016(2) -0.0012(18) 0.0055(17) 0.0007(19) Na3 0.078(3) 0.078(3) 0.074(4) 0.029(2) -0.029(2) -0.010(3) O1W 0.035(3) 0.058(4) 0.035(3) 0.008(2) -0.004(2) 0.006(3) O2W 0.032(3) 0.038(3) 0.066(4) -0.008(3) -0.002(3) -0.004(2) O3W 0.128(16) 0.119(15) 0.087(13) -0.019(11) -0.034(11) 0.038(12) O8W 0.109(10) 0.056(7) 0.034(6) -0.025(5) 0.000(6) 0.052(7) O9W 0.054(7) 0.100(9) 0.019(5) -0.022(5) -0.013(5) 0.032(7) O11W 0.111(11) 0.061(8) 0.089(10) -0.050(7) 0.032(8) -0.049(8) O12W 0.130(16) 0.061(12) 0.122(16) 0.000 -0.024(13) 0.000 O5W 0.125(13) 0.086(10) 0.105(11) -0.027(9) 0.045(10) 0.017(10) O10W 0.175(16) 0.115(13) 0.130(13) 0.030(11) -0.092(12) -0.061(12) O4W 0.043(11) 0.078(12) 0.042(11) 0.000 0.000 -0.010(9) O3WA 0.076(11) 0.156(17) 0.069(11) -0.028(11) -0.039(9) 0.021(12) O7W 0.099(15) 0.099(15) 0.093(19) 0.053(12) -0.053(12) -0.024(16) O13W 0.13(2) 0.15(2) 0.116(19) -0.064(16) 0.045(16) 0.011(17) O6W 0.11(2) 0.102(19) 0.15(2) -0.040(16) -0.005(17) -0.017(16) 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 O22 Mo3 Mo4 48.83(11) . . O22 Mo3 O23 86.57(15) . . O22 Mo3 O16 80.49(15) . . O22 Mo3 O26 160.88(16) . . O23 Mo3 Mo4 134.37(11) . . O23 Mo3 O16 72.83(14) . . O16 Mo3 Mo4 88.43(9) . . O26 Mo3 Mo4 135.99(11) . . O26 Mo3 O23 82.80(15) . . O26 Mo3 O16 81.20(14) . . O24 Mo3 Mo4 48.26(11) . . O24 Mo3 O22 95.39(15) . . O24 Mo3 O23 155.59(15) . . O24 Mo3 O16 83.47(15) . . O24 Mo3 O26 87.96(16) . . O25 Mo3 Mo4 100.29(15) . . O25 Mo3 O22 102.57(19) . . O25 Mo3 O23 98.34(18) . . O25 Mo3 O16 170.60(17) . . O25 Mo3 O26 94.69(18) . . O25 Mo3 O24 104.92(19) . . O15 Mo2 Mo1 49.09(11) . . O15 Mo2 O23 86.16(15) . . O15 Mo2 O16 79.96(15) . . O15 Mo2 O29 159.65(16) . . O23 Mo2 Mo1 134.72(11) . . O23 Mo2 O16 72.50(14) . . O16 Mo2 Mo1 90.50(9) . . O29 Mo2 Mo1 134.02(12) . . O29 Mo2 O23 85.01(15) . . O29 Mo2 O16 79.91(14) . . O5 Mo2 Mo1 48.39(11) 10_564 . O5 Mo2 O15 95.37(16) 10_564 . O5 Mo2 O23 156.99(16) 10_564 . O5 Mo2 O16 85.13(15) 10_564 . O5 Mo2 O29 85.84(16) 10_564 . O30 Mo2 Mo1 100.97(15) . . O30 Mo2 O15 103.31(19) . . O30 Mo2 O23 95.27(19) . . O30 Mo2 O16 167.24(18) . . O30 Mo2 O29 95.74(18) . . O30 Mo2 O5 106.6(2) . 10_564 O22 Mo4 Mo3 48.65(11) . . O22 Mo4 O17 82.42(15) . . O22 Mo4 O21 84.82(15) . . O22 Mo4 O31 160.76(16) . . O17 Mo4 Mo3 88.99(9) . . O21 Mo4 Mo3 132.55(11) . . O21 Mo4 O17 73.94(14) . . O21 Mo4 O31 83.40(16) . . O24 Mo4 Mo3 48.17(11) . . O24 Mo4 O22 95.13(15) . . O24 Mo4 O17 82.31(14) . . O24 Mo4 O21 156.07(16) . . O24 Mo4 O31 89.56(16) . . O31 Mo4 Mo3 137.52(12) . . O31 Mo4 O17 79.73(15) . . O33 Mo4 Mo3 99.13(14) 11_544 . O33 Mo4 O22 100.87(18) 11_544 . O33 Mo4 O17 171.44(17) 11_544 . O33 Mo4 O21 98.36(18) 11_544 . O33 Mo4 O24 105.11(18) 11_544 . O33 Mo4 O31 95.86(18) 11_544 . O15 Mo1 Mo2 48.88(11) . . O15 Mo1 O12 79.06(15) . . O15 Mo1 O13 87.16(16) . . O15 Mo1 O7 158.01(16) . . O12 Mo1 Mo2 88.02(10) . . O13 Mo1 Mo2 134.91(11) . . O13 Mo1 O12 71.76(14) . . O13 Mo1 O7 82.47(16) . . O5 Mo1 Mo2 48.47(12) 10_564 . O5 Mo1 O15 95.24(16) 10_564 . O5 Mo1 O12 82.75(15) 10_564 . O5 Mo1 O13 153.48(16) 10_564 . O5 Mo1 O7 85.79(17) 10_564 . O7 Mo1 Mo2 133.89(12) . . O7 Mo1 O12 79.29(14) . . O14 Mo1 Mo2 101.31(15) . . O14 Mo1 O15 104.82(19) . . O14 Mo1 O12 170.22(18) . . O14 Mo1 O13 99.25(19) . . O14 Mo1 O5 105.58(19) . 10_564 O14 Mo1 O7 95.99(19) . . O18 Mo6 Mo5 40.92(11) . . O18 Mo6 O12 81.47(15) . . O18 Mo6 O8 155.58(16) . . O12 Mo6 Mo5 85.54(10) . . O13 Mo6 Mo5 134.38(13) . . O13 Mo6 O18 94.56(17) . . O13 Mo6 O12 76.21(15) . . O13 Mo6 O8 91.16(17) . . O13 Mo6 O9 158.61(17) . . O8 Mo6 Mo5 125.11(11) . . O8 Mo6 O12 76.88(15) . . O9 Mo6 Mo5 40.05(11) . . O9 Mo6 O18 80.21(16) . . O9 Mo6 O12 82.50(15) . . O9 Mo6 O8 85.85(16) . . O10 Mo6 Mo5 98.56(16) . . O10 Mo6 O18 102.3(2) . . O10 Mo6 O12 175.77(19) . . O10 Mo6 O13 101.4(2) . . O10 Mo6 O8 99.8(2) . . O10 Mo6 O9 100.0(2) . . O18 Mo5 Mo6 41.00(11) . . O18 Mo5 O17 81.40(15) . . O18 Mo5 O19 160.63(16) . . O17 Mo5 Mo6 83.28(9) . . O21 Mo5 Mo6 132.63(12) . . O21 Mo5 O18 93.86(17) . . O21 Mo5 O17 74.36(15) . . O21 Mo5 O9 153.46(17) . . O21 Mo5 O19 88.40(17) . . O9 Mo5 Mo6 40.82(12) . . O9 Mo5 O18 81.05(16) . . O9 Mo5 O17 79.13(15) . . O9 Mo5 O19 88.35(17) . . O19 Mo5 Mo6 128.82(12) . . O19 Mo5 O17 80.70(14) . . O20 Mo5 Mo6 99.58(16) . . O20 Mo5 O18 100.90(19) . . O20 Mo5 O17 177.13(19) . . O20 Mo5 O21 103.7(2) . . O20 Mo5 O9 102.9(2) . . O20 Mo5 O19 97.23(19) . . O4 Fe1 O2 86.68(16) . . O4 Fe1 O1 173.02(17) . . O11 Fe1 O4 101.77(17) 10_564 . O11 Fe1 O2 167.80(17) 10_564 . O11 Fe1 O1 83.95(17) 10_564 . O3 Fe1 O4 90.89(16) . . O3 Fe1 O11 89.01(16) . 10_564 O3 Fe1 O2 82.00(17) . . O3 Fe1 O1 93.22(17) . . O2 Fe1 O1 88.31(16) . . O27 Fe1 O4 91.24(17) 10_564 . O27 Fe1 O11 98.52(16) 10_564 10_564 O27 Fe1 O3 171.58(18) 10_564 . O27 Fe1 O2 89.99(17) 10_564 . O27 Fe1 O1 83.90(18) 10_564 . O22 Fe2 O22 82.1(2) 5_556 . O15 Fe2 O22 84.97(14) . 5_556 O15 Fe2 O22 94.78(14) . . O15 Fe2 O22 94.78(14) 5_556 5_556 O15 Fe2 O22 84.97(14) 5_556 . O15 Fe2 O15 179.7(2) . 5_556 O18 Fe2 O22 179.13(14) . 5_556 O18 Fe2 O22 97.12(14) 5_556 5_556 O18 Fe2 O22 97.12(14) . . O18 Fe2 O22 179.13(14) 5_556 . O18 Fe2 O15 95.40(14) 5_556 5_556 O18 Fe2 O15 84.85(14) . 5_556 O18 Fe2 O15 84.84(14) 5_556 . O18 Fe2 O15 95.40(14) . . O18 Fe2 O18 83.7(2) . 5_556 O28 Fe3 O28 80.05(16) 11_544 19_576 O28 Fe3 O1W 83.42(19) 19_576 . O28 Fe3 O1W 80.85(18) 11_544 . O28 Fe3 O2W 92.45(18) 11_544 . O34 Fe3 O28 94.29(16) 28_656 19_576 O34 Fe3 O28 163.34(17) 28_656 11_544 O34 Fe3 O32 106.65(18) 28_656 . O34 Fe3 O1W 82.95(19) 28_656 . O34 Fe3 O2W 90.51(19) 28_656 . O32 Fe3 O28 89.50(17) . 11_544 O32 Fe3 O28 94.64(17) . 19_576 O32 Fe3 O1W 170.34(19) . . O32 Fe3 O2W 94.0(2) . . O2W Fe3 O28 168.5(2) . 19_576 O2W Fe3 O1W 86.8(2) . . O17 P3 O16 107.9(2) . . O17 P3 O12 108.5(2) . . O12 P3 O16 108.7(2) . . O11 P3 O16 110.3(2) . . O11 P3 O17 113.3(2) . . O11 P3 O12 108.1(2) . . O3 P1 O3 108.36(15) 28_656 10_564 O3 P1 O3 108.35(15) . 19_576 O3 P1 O3 111.7(3) 28_656 19_576 O3 P1 O3 108.35(15) . 28_656 O3 P1 O3 108.36(15) 19_576 10_564 O3 P1 O3 111.7(3) . 10_564 O26 P4 O28 107.7(2) . . O29 P4 O26 109.4(2) . . O29 P4 O28 107.7(2) . . O27 P4 O26 109.8(2) . . O27 P4 O28 109.1(2) . . O27 P4 O29 113.0(2) . . O2 P5 O19 107.0(2) 28_656 . O2 P5 O31 110.0(2) 28_656 . O2 P5 O32 111.9(3) 28_656 . O31 P5 O19 110.6(2) . . O32 P5 O19 107.7(2) . . O32 P5 O31 109.7(2) . . O4 P2 O8 109.1(2) . . O4 P2 O7 107.0(2) . . O7 P2 O8 110.8(2) . . O34 P2 O4 113.1(2) . . O34 P2 O8 108.5(2) . . O34 P2 O7 108.4(2) . . O8 Na1 O4 57.16(13) . . O9 Na1 O4 118.15(17) . . O9 Na1 O8 67.60(15) . . O9 Na1 O2 129.01(19) . . O3 Na1 O4 67.98(14) . . O3 Na1 O8 123.71(17) . . O3 Na1 O9 163.0(2) . . O3 Na1 O2 67.86(15) . . O3 Na1 O1 100.26(17) . 28_656 O2 Na1 O4 65.03(14) . . O2 Na1 O8 78.22(16) . . O1 Na1 O4 167.04(18) 28_656 . O1 Na1 O8 132.44(18) 28_656 . O1 Na1 O9 74.68(16) 28_656 . O1 Na1 O2 106.17(19) 28_656 . P2 Na2 Mo1 58.26(3) 10_564 10_564 Na2 Na2 Mo1 0(4) 10_564 10_564 Na2 Na2 P2 0(10) 10_564 10_564 Na2 Na2 O4 0(10) 10_564 10_564 Na2 Na2 O4 0(10) 10_564 . Na2 Na2 O5 0(10) 10_564 10_564 Na2 Na2 O5 0(10) 10_564 . Na2 Na2 O7 0(10) 10_564 . Na2 Na2 O7 0(10) 10_564 10_564 Na2 Na2 O4W 0(10) 10_564 . O4 Na2 Mo1 121.08(10) . 10_564 O4 Na2 Mo1 80.74(9) 10_564 10_564 O4 Na2 P2 28.19(9) 10_564 10_564 O4 Na2 P2 129.9(2) . 10_564 O4 Na2 O4 105.2(3) 10_564 . O4 Na2 O5 98.06(13) . . O4 Na2 O5 98.06(13) 10_564 10_564 O4 Na2 O5 105.22(14) . 10_564 O4 Na2 O5 105.22(14) 10_564 . O4 Na2 O7 144.62(19) . 10_564 O4 Na2 O7 56.85(12) . . O4 Na2 O7 56.85(12) 10_564 10_564 O4 Na2 O7 144.62(19) 10_564 . O4 Na2 O4W 127.40(13) . . O4 Na2 O4W 127.40(13) 10_564 . O5 Na2 Mo1 132.47(17) 10_564 10_564 O5 Na2 Mo1 29.64(9) . 10_564 O5 Na2 P2 86.96(9) . 10_564 O5 Na2 P2 100.59(9) 10_564 10_564 O5 Na2 O5 141.3(3) . 10_564 O5 Na2 O7 107.33(15) 10_564 10_564 O5 Na2 O7 63.61(13) . 10_564 O5 Na2 O7 107.33(15) . . O5 Na2 O7 63.61(13) 10_564 . O5 Na2 O4W 70.64(14) . . O5 Na2 O4W 70.64(14) 10_564 . O7 Na2 Mo1 34.11(9) 10_564 10_564 O7 Na2 Mo1 134.32(15) . 10_564 O7 Na2 P2 29.13(9) 10_564 10_564 O7 Na2 P2 163.87(9) . 10_564 O7 Na2 O7 154.5(3) 10_564 . O4W Na2 Mo1 73.00(8) . 10_564 O4W Na2 P2 101.36(10) . 10_564 O4W Na2 O7 77.23(14) . . O4W Na2 O7 77.23(14) . 10_564 Mo3 O22 Mo4 82.52(15) . . Mo3 O22 Fe2 134.44(19) . . Mo4 O22 Fe2 133.74(19) . . Mo2 O15 Mo1 82.03(15) . . Mo2 O15 Fe2 135.5(2) . . Mo1 O15 Fe2 135.37(19) . . Mo6 O18 Fe2 128.56(19) . . Mo5 O18 Mo6 98.08(17) . . Mo5 O18 Fe2 126.90(19) . . Mo3 O23 Mo2 111.94(17) . . Mo2 O16 Mo3 101.92(14) . . P3 O16 Mo3 127.4(2) . . P3 O16 Mo2 124.9(2) . . Mo4 O17 Mo5 91.37(13) . . P3 O17 Mo4 126.1(2) . . P3 O17 Mo5 129.7(2) . . Mo6 O12 Mo1 93.72(14) . . P3 O12 Mo1 125.4(2) . . P3 O12 Mo6 132.7(2) . . P4 O26 Mo3 129.2(2) . . Mo6 O13 Mo1 117.95(19) . . Mo5 O21 Mo4 119.8(2) . . Fe3 O28 Fe3 99.95(16) 12_454 28_656 P4 O28 Fe3 135.6(2) . 12_454 P4 O28 Fe3 121.5(2) . 28_656 Mo3 O24 Mo4 83.57(14) . . Fe1 O4 Na1 80.46(14) . . Fe1 O4 Na2 116.99(18) . . Fe1 O4 Na2 116.99(18) . 10_564 P2 O4 Fe1 132.1(2) . . P2 O4 Na1 93.52(19) . . P2 O4 Na2 102.4(2) . 10_564 P2 O4 Na2 102.4(2) . . Na2 O4 Na1 131.59(18) . . Na2 O4 Na1 131.59(18) 10_564 . Na2 O4 Na2 0.00(19) 10_564 . P4 O29 Mo2 130.1(2) . . Mo6 O8 Na1 96.67(16) . . P2 O8 Mo6 133.5(2) . . P2 O8 Na1 100.2(2) . . Mo6 O9 Na1 104.90(18) . . Mo5 O9 Mo6 99.13(18) . . Mo5 O9 Na1 141.9(2) . . P3 O11 Fe1 137.9(2) . 10_564 Fe1 O3 Na1 94.75(16) . . P1 O3 Fe1 143.9(2) . . P1 O3 Na1 118.6(2) . . Mo2 O5 Na2 161.9(2) 10_564 . Mo2 O5 Na2 161.9(2) 10_564 10_564 Mo1 O5 Mo2 83.13(16) 10_564 10_564 Mo1 O5 Na2 111.01(17) 10_564 10_564 Mo1 O5 Na2 111.01(17) 10_564 . Na2 O5 Na2 0.0(2) . 10_564 Mo1 O7 Na2 99.24(16) . . Mo1 O7 Na2 99.24(16) . 10_564 P2 O7 Mo1 135.0(2) . . P2 O7 Na2 92.1(2) . . P2 O7 Na2 92.1(2) . 10_564 Na2 O7 Na2 0.0(2) 10_564 . P2 O34 Fe3 145.1(3) . 19_576 Fe1 O2 Na1 88.93(16) . . P5 O2 Fe1 135.4(2) 19_576 . P5 O2 Na1 135.7(2) 19_576 . P5 O19 Mo5 134.2(2) . . P4 O27 Fe1 166.2(3) . 10_564 Fe1 O1 Na1 114.5(2) . 19_576 P5 O31 Mo4 137.5(2) . . P5 O32 Fe3 142.6(3) . . Mo4 O33 Na3 147.1(3) 12_454 . Mo2 O30 Na3 144.9(3) . . O33 Na3 O33 115.4(3) . 15_445 O33 Na3 O30 83.86(14) 15_445 . O33 Na3 O30 83.86(14) . 15_445 O33 Na3 O30 146.50(15) . . O33 Na3 O30 146.50(15) 15_445 15_445 O33 Na3 O3W 75.1(5) . 15_445 O33 Na3 O3W 75.1(5) 15_445 . O33 Na3 O3W 76.1(5) 15_445 15_445 O33 Na3 O3W 76.1(5) . . O30 Na3 O30 94.3(3) . 15_445 O30 Na3 O3W 84.2(5) . 15_445 O30 Na3 O3W 84.2(5) 15_445 . O30 Na3 O3W 137.2(5) 15_445 15_445 O30 Na3 O3W 137.2(5) . . O3W Na3 O3W 124.6(11) . 15_445 O3WA Na3 O33 76.0(5) 15_445 . O3WA Na3 O33 91.3(7) 15_445 15_445 O3WA Na3 O33 91.3(7) . . O3WA Na3 O33 76.0(5) . 15_445 O3WA Na3 O30 120.8(7) 15_445 15_445 O3WA Na3 O30 76.5(5) . 15_445 O3WA Na3 O30 76.5(5) 15_445 . O3WA Na3 O30 120.8(7) . . O3WA Na3 O3W 139.6(8) . 15_445 O3WA Na3 O3W 17.8(8) 15_445 15_445 O3WA Na3 O3WA 156.3(13) . 15_445 Na2 O4W Na2 0.0 10_564 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Mo3 Mo4 2.5994(7) . Mo3 O22 1.968(4) . Mo3 O23 2.090(4) . Mo3 O16 2.250(4) . Mo3 O26 2.069(4) . Mo3 O24 1.949(4) . Mo3 O25 1.682(4) . Mo2 Mo1 2.5757(7) . Mo2 O15 1.959(4) . Mo2 O23 2.119(4) . Mo2 O16 2.241(4) . Mo2 O29 2.077(4) . Mo2 O5 1.942(4) 10_564 Mo2 O30 1.687(4) . Mo4 O22 1.974(4) . Mo4 O17 2.280(4) . Mo4 O21 2.049(4) . Mo4 O24 1.952(4) . Mo4 O31 2.064(4) . Mo4 O33 1.679(4) 11_544 Mo1 O15 1.966(4) . Mo1 O12 2.296(4) . Mo1 O13 2.069(4) . Mo1 O5 1.940(4) 10_564 Mo1 O7 2.080(4) . Mo1 O14 1.674(4) . Mo6 Mo5 2.9584(7) . Mo6 O18 1.960(4) . Mo6 O12 2.286(4) . Mo6 O13 1.830(4) . Mo6 O8 2.017(4) . Mo6 O9 1.959(4) . Mo6 O10 1.681(4) . Mo5 O18 1.957(4) . Mo5 O17 2.416(4) . Mo5 O21 1.834(4) . Mo5 O9 1.928(4) . Mo5 O19 2.020(4) . Mo5 O20 1.671(4) . Fe1 O4 2.001(4) . Fe1 O11 1.968(4) 10_564 Fe1 O3 1.939(4) . Fe1 O2 2.017(4) . Fe1 O27 1.922(4) 10_564 Fe1 O1 2.146(4) . Fe2 O22 2.189(4) . Fe2 O22 2.189(4) 5_556 Fe2 O15 2.179(4) . Fe2 O15 2.179(4) 5_556 Fe2 O18 2.172(4) 5_556 Fe2 O18 2.172(4) . Fe3 O28 2.085(4) 11_544 Fe3 O28 2.113(4) 19_576 Fe3 O34 1.953(4) 28_656 Fe3 O32 1.990(5) . Fe3 O1W 2.200(5) . Fe3 O2W 2.097(5) . P3 O16 1.553(4) . P3 O17 1.539(4) . P3 O12 1.544(4) . P3 O11 1.517(4) . P1 O3 1.527(4) 28_656 P1 O3 1.527(4) 10_564 P1 O3 1.527(4) 19_576 P1 O3 1.527(4) . P4 O26 1.549(4) . P4 O28 1.550(4) . P4 O29 1.531(4) . P4 O27 1.503(4) . P5 O2 1.507(4) 28_656 P5 O19 1.568(4) . P5 O31 1.539(4) . P5 O32 1.528(4) . P2 O4 1.524(4) . P2 O8 1.562(4) . P2 O7 1.535(4) . P2 O34 1.514(4) . Na1 O4 2.717(5) . Na1 O8 2.526(5) . Na1 O9 2.333(5) . Na1 O3 2.259(5) . Na1 O2 2.387(5) . Na1 O1 2.332(5) 28_656 Na2 Na2 0.000(10) 10_564 Na2 O4 2.449(5) . Na2 O4 2.449(5) 10_564 Na2 O5 2.487(4) 10_564 Na2 O5 2.487(4) . Na2 O7 2.698(4) . Na2 O7 2.698(4) 10_564 Na2 O4W 2.64(3) . O33 Na3 2.444(5) . O30 Na3 2.462(6) . Na3 O3W 2.80(3) 15_445 Na3 O3W 2.80(3) . Na3 O3WA 2.34(2) 15_445 Na3 O3WA 2.34(2) . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_4 Mo1 Mo2 O30 Na3 152.2(4) . . Mo6 Mo5 O21 Mo4 -71.4(3) . . Mo5 Mo6 O13 Mo1 74.7(2) . . O15 Mo2 O30 Na3 102.0(4) . . O18 Mo6 O13 Mo1 85.3(2) . . O18 Mo5 O21 Mo4 -86.4(2) . . O23 Mo2 O30 Na3 14.7(4) . . O16 Mo2 O30 Na3 -1.5(11) . . O16 P3 O17 Mo4 -10.3(3) . . O16 P3 O17 Mo5 119.7(3) . . O16 P3 O12 Mo1 16.5(3) . . O16 P3 O12 Mo6 -123.2(3) . . O16 P3 O11 Fe1 14.9(4) . 10_564 O17 Mo5 O21 Mo4 -6.45(19) . . O17 P3 O16 Mo3 13.2(3) . . O17 P3 O16 Mo2 -135.2(2) . . O17 P3 O12 Mo1 133.6(2) . . O17 P3 O12 Mo6 -6.1(4) . . O17 P3 O11 Fe1 -106.1(4) . 10_564 O12 Mo6 O13 Mo1 5.29(19) . . O12 P3 O16 Mo3 130.8(2) . . O12 P3 O16 Mo2 -17.6(3) . . O12 P3 O17 Mo4 -128.0(2) . . O12 P3 O17 Mo5 2.0(3) . . O12 P3 O11 Fe1 133.6(4) . 10_564 O26 P4 O28 Fe3 -10.0(4) . 12_454 O26 P4 O28 Fe3 146.4(2) . 28_656 O26 P4 O29 Mo2 -47.0(4) . . O26 P4 O27 Fe1 91.4(12) . 10_564 O28 P4 O26 Mo3 169.3(3) . . O28 P4 O29 Mo2 -163.9(3) . . O28 P4 O27 Fe1 -150.8(12) . 10_564 O4 P2 O8 Mo6 107.8(3) . . O4 P2 O8 Na1 -1.7(2) . . O4 P2 O7 Mo1 -94.2(4) . . O4 P2 O7 Na2 11.1(2) . 10_564 O4 P2 O7 Na2 11.1(2) . . O4 P2 O34 Fe3 88.9(5) . 19_576 O29 Mo2 O30 Na3 -70.8(4) . . O29 P4 O26 Mo3 52.5(4) . . O29 P4 O28 Fe3 -95.7(3) . 28_656 O29 P4 O28 Fe3 107.9(3) . 12_454 O29 P4 O27 Fe1 -31.0(13) . 10_564 O8 Mo6 O13 Mo1 -70.9(2) . . O8 P2 O4 Fe1 81.9(3) . . O8 P2 O4 Na1 1.6(2) . . O8 P2 O4 Na2 -132.4(2) . . O8 P2 O4 Na2 -132.4(2) . 10_564 O8 P2 O7 Mo1 24.6(4) . . O8 P2 O7 Na2 129.9(2) . 10_564 O8 P2 O7 Na2 129.9(2) . . O8 P2 O34 Fe3 -32.3(5) . 19_576 O9 Mo6 O13 Mo1 10.7(6) . . O9 Mo5 O21 Mo4 -8.7(5) . . O11 P3 O16 Mo3 -110.9(3) . . O11 P3 O16 Mo2 100.7(3) . . O11 P3 O17 Mo4 112.0(3) . . O11 P3 O17 Mo5 -118.0(3) . . O11 P3 O12 Mo1 -103.2(3) . . O11 P3 O12 Mo6 117.1(3) . . O3 P1 O3 Fe1 -178.1(5) 28_656 . O3 P1 O3 Fe1 -56.7(3) 19_576 . O3 P1 O3 Fe1 62.6(4) 10_564 . O3 P1 O3 Na1 148.1(3) 19_576 . O3 P1 O3 Na1 26.71(18) 28_656 . O3 P1 O3 Na1 -92.6(2) 10_564 . O5 Mo2 O30 Na3 -158.2(4) 10_564 . O7 P2 O4 Fe1 -158.2(3) . . O7 P2 O4 Na1 121.5(2) . . O7 P2 O4 Na2 -12.5(2) . 10_564 O7 P2 O4 Na2 -12.5(2) . . O7 P2 O8 Mo6 -9.8(4) . . O7 P2 O8 Na1 -119.3(2) . . O7 P2 O34 Fe3 -152.6(4) . 19_576 O34 P2 O4 Fe1 -39.0(4) . . O34 P2 O4 Na1 -119.3(2) . . O34 P2 O4 Na2 106.7(2) . 10_564 O34 P2 O4 Na2 106.7(2) . . O34 P2 O8 Mo6 -128.6(3) . . O34 P2 O8 Na1 121.9(2) . . O34 P2 O7 Mo1 143.6(3) . . O34 P2 O7 Na2 -111.2(2) . . O34 P2 O7 Na2 -111.2(2) . 10_564 O2 P5 O19 Mo5 -114.2(3) 28_656 . O2 P5 O31 Mo4 108.7(4) 28_656 . O2 P5 O32 Fe3 6.8(5) 28_656 . O19 Mo5 O21 Mo4 74.3(2) . . O19 P5 O31 Mo4 -9.3(4) . . O19 P5 O32 Fe3 124.1(4) . . O27 P4 O26 Mo3 -72.1(3) . . O27 P4 O28 Fe3 27.3(3) . 28_656 O27 P4 O28 Fe3 -129.1(3) . 12_454 O27 P4 O29 Mo2 75.6(4) . . O31 P5 O19 Mo5 5.6(4) . . O31 P5 O32 Fe3 -115.6(4) . . O32 P5 O19 Mo5 125.4(3) . . O32 P5 O31 Mo4 -127.8(4) . . O20 Mo5 O21 Mo4 171.4(2) . . O10 Mo6 O13 Mo1 -171.1(2) . .