#------------------------------------------------------------------------------ #$Date: 2016-08-07 11:36:57 +0300 (Sun, 07 Aug 2016) $ #$Revision: 185288 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/45/7224542.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_7224542 loop_ _publ_author_name 'Reddy, Pulikanti Guruprasad' 'Mamidi, Narsimha' 'Pradeep, Chullikkattil P.' _publ_section_title ; An organic--inorganic hybrid supramolecular framework material based on a [P2W18O62]6−cluster and Yb & Na complexes of pyridine-2,6-dicarboxylic acid: a catalyst for selective oxidation of sulfides in water with H2O2 ; _journal_issue 23 _journal_name_full CrystEngComm _journal_page_first 4272 _journal_paper_doi 10.1039/C5CE02546J _journal_volume 18 _journal_year 2016 _chemical_formula_moiety 'C28 H40 N4 Na2 O58 P W9 Yb' _chemical_formula_sum 'C28 H40 N4 Na2 O58 P W9 Yb' _chemical_formula_weight 3265.28 _chemical_name_systematic 'Chemistry DepartmentAMRCIIT MandiHimachal Pradesh175001' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2014 _audit_update_record ; 2015-12-24 deposited with the CCDC. 2016-03-04 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 101.071(8) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 18.2405(16) _cell_length_b 35.036(2) _cell_length_c 22.8447(14) _cell_measurement_reflns_used 5329 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 27.9200 _cell_measurement_theta_min 2.3550 _cell_volume 14327.8(18) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET) (compiled Apr 11 2014,15:12:41) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET) (compiled Apr 11 2014,15:12:41) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET) (compiled Apr 11 2014,15:12:41) ; _computing_molecular_graphics 'Ortep for Windows (Farrugia, 2012)' _computing_publication_material 'WinGX publication routines (Farrugia, 2012)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_structure_solution 'SHELXL-2014 (Sheldrick, 2014) and OlEX2' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.868 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_unetI/netI 0.0903 _diffrn_reflns_Laue_measured_fraction_full 0.989 _diffrn_reflns_Laue_measured_fraction_max 0.868 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 23691 _diffrn_reflns_point_group_measured_fraction_full 0.989 _diffrn_reflns_point_group_measured_fraction_max 0.868 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.401 _diffrn_reflns_theta_min 1.817 _diffrn_source 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 15.827 _exptl_absorpt_correction_T_max 0.292 _exptl_absorpt_correction_T_min 0.016 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET) (compiled Apr 11 2014,15:12:41) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour white _exptl_crystal_density_diffrn 3.027 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 11784 _exptl_crystal_size_max 0.4668 _exptl_crystal_size_mid 0.0692 _exptl_crystal_size_min 0.0437 _refine_diff_density_max 7.785 _refine_diff_density_min -4.047 _refine_diff_density_rms 0.657 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 864 _refine_ls_number_reflns 15635 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.048 _refine_ls_R_factor_all 0.1233 _refine_ls_R_factor_gt 0.0849 _refine_ls_shift/su_max 0.197 _refine_ls_shift/su_mean 0.065 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1626P)^2^+1120.9960P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2288 _refine_ls_wR_factor_ref 0.2872 _reflns_Friedel_coverage 0.000 _reflns_number_gt 10879 _reflns_number_total 15635 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c5ce02546j2.cif _cod_data_source_block shelx _cod_depositor_comments 'Adding full bibliography for 7224542.cif.' _cod_original_cell_volume 14327.7(18) _cod_database_code 7224542 _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. ; _shelxl_version_number 2014-3 _shelx_res_file ; TITL CF solution in C2/c CELL 0.71073 18.2405 35.0359 22.8447 90.000 101.071 90.000 ZERR 8.00 0.0016 0.0023 0.0014 0.000 0.008 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O P W NA YB UNIT 224 320 32 464 8 72 16 8 MERG 2 DFIX 0.85 0.01 O41 HC DANG 2.127839 0.02 W7 Hc FMAP 2 PLAN 20 BOND $H CONF ACTA HTAB L.S. 10 EQIV $1 -x, y, -z+1/2 HTAB O35 O39_$1 EQIV $2 -x-1/2, -y+3/2, -z+1 HTAB O33 O49_$2 EQIV $3 x-1, y, z HTAB O37 O52_$3 EQIV $4 -x+1, y, -z+1/2 HTAB O39 O58_$4 HTAB O39 O53_$4 EQIV $5 -x+1/2, -y+3/2, -z+1 HTAB O29 O43_$5 HTAB C12 O19_$2 HTAB C19 O51_$5 HTAB C3 O40_$5 EQIV $6 x+1, y, z HTAB O55 O5_$6 HTAB O55 O44_$6 HTAB C26 O41 HTAB O58 O35_$6 HTAB O58 O39_$4 HTAB O56 O40_$6 EQIV $7 -x+2, y, -z+1/2 HTAB O56 O53_$7 HTAB O56 O39_$4 HTAB O54 O43 EQIV $8 x-1/2, y-1/2, z HTAB O47 O37_$8 HTAB O53 O58 HTAB O53 O56_$7 EQIV $9 x+1/2, -y+3/2, z-1/2 HTAB O53 O29_$9 EQIV $10 -x+1, -y+1, -z+1 HTAB O57 O27_$10 EQIV $11 x+1, -y+1, z-1/2 HTAB O57 O2_$11 HTAB O57 O28_$10 HTAB O52 O4_$5 HTAB O52 O49_$5 WGHT 0.162600 1120.995972 FVAR 0.26158 W6 6 0.012927 0.579363 0.580278 11.00000 0.03102 0.02466 = 0.02096 -0.00153 0.01079 0.00120 W5 6 -0.045820 0.670014 0.637517 11.00000 0.03426 0.01936 = 0.02181 0.00192 0.00968 0.00112 W4 6 -0.134965 0.669880 0.753706 11.00000 0.03283 0.02212 = 0.02425 -0.00209 0.01056 0.00433 W8 6 0.193191 0.579687 0.689025 11.00000 0.02769 0.03079 = 0.02367 -0.00175 0.01099 0.00023 W7 6 -0.041818 0.496988 0.632394 11.00000 0.03763 0.01978 = 0.02596 -0.00454 0.00877 0.00084 W1 6 -0.185744 0.607587 0.548496 11.00000 0.03233 0.02826 = 0.02317 -0.00031 0.00648 0.00343 W9 6 0.139175 0.497052 0.740977 11.00000 0.03572 0.02207 = 0.02807 -0.00188 0.00871 0.00497 W2 6 -0.282117 0.611643 0.660248 11.00000 0.02888 0.03296 = 0.02592 -0.00140 0.00766 0.00393 W3 6 -0.237828 0.526114 0.608646 11.00000 0.03422 0.02911 = 0.02807 -0.00273 0.00390 -0.00322 YB1 8 0.026810 0.789538 0.445522 11.00000 0.03927 0.03236 = 0.02773 0.00328 0.01014 0.00412 P1 5 -0.094389 0.582115 0.692970 11.00000 0.02789 0.00461 = 0.01432 0.00042 0.01156 -0.00062 O17 4 -0.037878 0.561738 0.663653 11.00000 0.04329 0.01443 = 0.02424 0.00821 0.00955 0.00350 O23 4 0.252439 0.585708 0.641262 11.00000 0.03348 O7 4 -0.170521 0.581465 0.646651 11.00000 0.05031 0.01585 = 0.01958 0.01067 0.00641 0.00158 O15 4 0.043693 0.586503 0.516008 11.00000 0.04708 0.02093 = 0.07027 -0.02452 0.03970 -0.00944 O14 4 0.006412 0.629024 0.608981 11.00000 0.02815 0.03196 = 0.01559 -0.00442 0.00364 -0.00085 O3 4 -0.270538 0.624506 0.582854 11.00000 0.04653 0.03815 = 0.01986 -0.01142 0.00785 -0.01037 O20 4 0.102906 0.571686 0.630398 11.00000 0.04897 0.02189 = 0.02865 -0.00195 0.02468 0.00352 O9 4 -0.097354 0.586677 0.545301 11.00000 0.02565 O25 4 0.199980 0.526118 0.697542 11.00000 0.03343 0.03362 = 0.03200 -0.00545 0.02100 0.00267 O36 4 -0.063804 0.783129 0.352766 11.00000 0.02422 0.04643 = 0.03547 0.00668 0.00148 0.00989 O40 4 0.089431 0.763284 0.376386 11.00000 0.04026 0.03551 = 0.02346 -0.00608 0.00331 -0.00490 O10 4 -0.132636 0.649139 0.589223 11.00000 0.03289 0.02028 = 0.01948 -0.00448 0.00448 -0.00086 O35 4 -0.179932 0.778568 0.305206 11.00000 0.03626 0.03385 = 0.02580 0.00786 -0.00137 0.00066 AFIX 83 H35 2 -0.160898 0.777230 0.275540 11.00000 -1.50000 AFIX 0 O19 4 -0.102328 0.695259 0.689156 11.00000 0.03457 0.01561 = 0.02022 0.00535 0.00327 -0.00178 O21 4 0.058570 0.497864 0.678720 11.00000 0.03739 0.02384 = 0.03525 -0.00505 0.01013 0.00648 O8 4 -0.219643 0.649882 0.696033 11.00000 0.03961 0.02749 = 0.02938 -0.00988 0.01929 -0.00341 O31 4 -0.001149 0.666029 0.466621 11.00000 0.06712 0.04913 = 0.08791 0.00592 0.01466 -0.01196 O27 4 0.212267 0.508834 0.812302 11.00000 0.03638 0.02921 = 0.05321 0.00807 0.02292 0.00668 O41 4 0.038982 0.548000 0.395646 11.00000 0.06101 0.02368 = 0.02707 -0.00699 0.01109 0.00433 O16 4 -0.007708 0.525054 0.573904 11.00000 0.03819 0.02592 = 0.02835 0.00059 0.01140 0.00854 O1 4 -0.294332 0.490703 0.575786 11.00000 0.03294 0.04233 = 0.03592 -0.01039 0.00415 -0.01674 O22 4 0.155744 0.629251 0.698658 11.00000 0.04467 0.03040 = 0.01146 -0.00767 -0.00036 -0.01001 O5 4 -0.209364 0.625028 0.478416 11.00000 0.05000 0.02626 = 0.02875 0.00730 0.00782 0.00951 O28 4 0.260401 0.587403 0.762152 11.00000 0.03004 0.05297 = 0.03499 0.00281 0.01800 0.01326 O13 4 0.041533 0.676127 0.698131 11.00000 0.02835 0.01793 = 0.02152 0.00259 0.00640 -0.00066 N3 3 0.058631 0.834931 0.373116 11.00000 0.03590 0.04601 = 0.03594 0.00555 0.00177 0.00338 O2 4 -0.310256 0.560429 0.629671 11.00000 0.03302 0.03720 = 0.03669 0.00219 0.00536 -0.00419 O18 4 -0.073474 0.487985 0.706660 11.00000 0.02552 O26 4 0.171265 0.451978 0.732257 11.00000 0.04728 0.03539 = 0.03133 0.00321 0.00265 0.02082 NA1 7 0.038328 0.613633 0.421597 11.00000 0.24885 0.04448 = 0.04099 -0.00598 0.01700 0.00820 O33 4 -0.062911 0.809386 0.608919 11.00000 0.06686 0.09612 = 0.03283 0.00633 0.02877 0.01301 AFIX 83 H33 2 -0.107042 0.814375 0.607987 11.00000 -1.50000 AFIX 0 O12 4 -0.031664 0.706921 0.593194 11.00000 0.06228 0.01729 = 0.01741 0.00376 0.01465 -0.00357 O6 4 -0.141842 0.509614 0.598312 11.00000 0.03861 0.03073 = 0.02175 -0.00070 -0.00557 0.00242 O37 4 -0.015944 0.914891 0.430739 11.00000 0.07385 0.03624 = 0.05922 0.00105 0.03523 -0.00247 AFIX 83 H37 2 -0.036415 0.916587 0.459606 11.00000 -1.50000 AFIX 0 N2 3 -0.103667 0.790333 0.454526 11.00000 0.02697 0.03344 = 0.02366 -0.00314 0.00628 0.00669 O32 4 -0.015308 0.726654 0.442216 11.00000 0.03503 0.03804 = 0.03724 -0.00771 0.00047 -0.00930 O34 4 0.009060 0.794088 0.544754 11.00000 0.06701 0.04922 = 0.02806 0.00551 0.01479 0.01292 O38 4 -0.008499 0.853288 0.459511 11.00000 0.06739 0.02641 = 0.04357 0.00040 0.02130 0.00530 O39 4 0.137744 0.765477 0.293029 11.00000 0.04245 0.05219 = 0.03082 -0.00245 0.01602 0.00971 AFIX 83 H39 2 0.144213 0.742723 0.300728 11.00000 -1.50000 AFIX 0 N1 3 0.111718 0.744890 0.505173 11.00000 0.02732 O4 4 -0.235149 0.559072 0.540229 11.00000 0.02265 0.03793 = 0.02690 -0.01107 0.00285 0.00280 O30 4 0.138732 0.816776 0.489491 11.00000 0.06265 0.04775 = 0.03502 -0.00880 0.00084 -0.01314 C9 1 -0.120840 0.795190 0.508694 11.00000 0.07505 0.03076 = 0.02149 -0.00536 0.01839 -0.01679 O29 4 0.246959 0.815373 0.556987 11.00000 0.08128 0.05110 = 0.07637 0.00981 -0.01051 -0.03251 AFIX 83 H29 2 0.247497 0.838045 0.548171 11.00000 -1.50000 AFIX 0 C12 1 -0.234226 0.786749 0.411986 11.00000 0.03792 0.03596 = 0.04648 0.01396 0.00510 0.00941 AFIX 43 H12 2 -0.272480 0.783418 0.379053 11.00000 -1.20000 AFIX 0 C10 1 -0.193777 0.796464 0.517138 11.00000 0.07411 0.02059 = 0.01942 0.00780 0.00729 0.00610 AFIX 43 H10 2 -0.204411 0.800120 0.554959 11.00000 -1.20000 AFIX 0 C13 1 -0.157428 0.786459 0.406500 11.00000 0.07266 0.01076 = 0.05683 0.00126 0.02603 -0.00125 C18 1 0.091710 0.884724 0.288171 11.00000 0.04750 0.05515 = 0.04114 0.03000 0.01482 0.01456 AFIX 43 H18 2 0.102625 0.901872 0.259970 11.00000 -1.20000 AFIX 0 C6 1 0.091990 0.709424 0.508822 11.00000 0.04601 0.03921 = 0.03721 -0.00099 0.02134 0.00721 C2 1 0.175432 0.758579 0.537958 11.00000 0.02571 0.03840 = 0.03440 0.00674 -0.00787 0.00277 C5 1 0.136018 0.684586 0.547938 11.00000 0.05180 0.02616 = 0.06346 0.01627 0.02528 0.00579 AFIX 43 H5 2 0.121749 0.659308 0.551166 11.00000 -1.20000 AFIX 0 C11 1 -0.249094 0.792282 0.469244 11.00000 0.07286 0.03530 = 0.05569 0.01941 0.04970 0.01617 AFIX 43 H11 2 -0.298442 0.793091 0.474343 11.00000 -1.20000 AFIX 0 C4 1 0.200250 0.698042 0.581287 11.00000 0.05307 0.06776 = 0.06251 0.02985 0.01841 0.01557 AFIX 43 H4 2 0.231297 0.681759 0.607065 11.00000 -1.20000 AFIX 0 C1 1 0.187394 0.799944 0.528301 11.00000 0.07072 0.03694 = 0.03816 -0.00398 0.00541 0.00483 C19 1 0.109089 0.847523 0.285653 11.00000 0.03762 0.05882 = 0.02966 0.01638 -0.00509 -0.01163 AFIX 43 H19 2 0.133085 0.838806 0.255792 11.00000 -1.20000 AFIX 0 O11 4 -0.073833 0.623734 0.705777 11.00000 0.03260 0.02055 = 0.02212 -0.00176 0.01544 -0.00333 O24 4 0.109611 0.561328 0.751755 11.00000 0.01870 0.02944 = 0.01018 -0.00958 0.00085 0.00015 C21 1 0.108307 0.780976 0.332043 11.00000 0.01898 0.04182 = 0.02364 0.00572 -0.00843 0.01347 C8 1 -0.054730 0.797763 0.558311 11.00000 0.05908 0.05213 = 0.04140 0.00163 0.02815 0.02197 C7 1 0.021512 0.699522 0.469368 11.00000 0.03892 0.04166 = 0.05345 0.02139 0.01542 0.00668 C20 1 0.091038 0.821593 0.328210 11.00000 0.04519 0.02353 = 0.03657 0.00904 0.01681 0.02203 C14 1 -0.128729 0.783793 0.351544 11.00000 0.05246 0.02235 = 0.04897 0.00852 0.02102 0.00215 C15 1 0.003959 0.880121 0.424906 11.00000 0.04693 0.03909 = 0.03843 0.02192 0.00504 0.02159 C3 1 0.219739 0.735787 0.577139 11.00000 0.04689 0.05943 = 0.03198 0.00297 0.02040 0.00842 AFIX 43 H3 2 0.262852 0.745393 0.601037 11.00000 -1.20000 AFIX 0 C17 1 0.056960 0.896902 0.334083 11.00000 0.04092 0.03852 = 0.08385 0.00021 0.02750 -0.01001 AFIX 43 H17 2 0.044015 0.922472 0.336160 11.00000 -1.20000 AFIX 0 C16 1 0.041446 0.871902 0.376322 11.00000 0.06082 0.01622 = 0.05049 -0.00053 0.00258 -0.00256 O43 4 0.172139 0.612336 0.440058 11.00000 0.13636 0.15181 = 0.18136 0.02588 0.06207 -0.06169 O44 4 -0.105048 0.607765 0.382159 11.00000 0.15677 0.09757 = 0.18057 -0.02234 0.08208 -0.03491 O50 4 0.181176 0.707015 0.720376 11.00000 0.04440 0.02518 = 0.04191 0.00643 0.01651 -0.01149 O51 4 0.367145 0.629834 0.838239 11.00000 0.01819 0.05996 = 0.03187 -0.01821 -0.00029 -0.00280 C22 1 -0.349837 0.496033 0.399749 11.00000 0.14097 AFIX 6 O55 4 0.842266 0.692092 0.418548 11.00000 0.06050 0.13982 = 0.16995 0.01961 0.04460 0.00084 H55A 2 0.856922 0.669054 0.419060 11.00000 -1.50000 H55B 2 0.839472 0.701253 0.383723 11.00000 -1.50000 AFIX 0 C26 1 -0.131337 0.533918 0.433558 11.00000 0.07098 AFIX 43 H26 2 -0.082267 0.542550 0.439198 11.00000 -1.20000 AFIX 6 O58 4 0.832367 0.694373 0.231054 11.00000 0.20702 0.21846 = 0.05183 0.03694 0.02675 -0.08141 H58A 2 0.840057 0.712785 0.208766 11.00000 -1.50000 H58B 2 0.823719 0.674148 0.210338 11.00000 -1.50000 AFIX 0 C24 1 -0.220785 0.488720 0.447901 11.00000 0.06329 AFIX 43 H24 2 -0.235012 0.465984 0.463528 11.00000 -1.20000 AFIX 0 O45 4 -0.231576 0.609185 0.338436 11.00000 0.16944 0.11292 = 0.08855 0.01091 0.01446 0.06263 AFIX 6 O56 4 0.958390 0.705101 0.296774 11.00000 0.14253 0.09262 = 0.10113 -0.03770 0.01203 0.01860 H56A 2 0.940656 0.713599 0.326022 11.00000 -1.50000 H56B 2 0.993290 0.719691 0.290448 11.00000 -1.50000 AFIX 0 C25 1 -0.143811 0.502651 0.459282 11.00000 0.06188 AFIX 43 H25 2 -0.105665 0.489484 0.483996 11.00000 -1.20000 AFIX 0 N4 3 -0.257730 0.542693 0.387104 11.00000 0.08300 AFIX 6 O54 4 0.331030 0.592626 0.508863 11.00000 0.72070 0.92920 = 0.53107 0.68589 -0.40000 -0.40000 H54A 2 0.285455 0.587539 0.508781 11.00000 -1.50000 H54B 2 0.358702 0.579516 0.535680 11.00000 -1.50000 AFIX 0 C23 1 -0.268587 0.511632 0.413077 11.00000 0.07602 O47 4 -0.367746 0.472040 0.434486 11.00000 0.14105 0.24665 = 0.10243 0.00348 0.02411 -0.07487 AFIX 83 H47 2 -0.411689 0.466108 0.423280 11.00000 -1.50000 AFIX 0 O46 4 -0.400996 0.519755 0.363488 11.00000 0.03955 0.11023 = 0.05947 0.00357 -0.00050 0.01556 C27 1 -0.185135 0.555451 0.398420 11.00000 0.07794 C28 1 -0.171999 0.593299 0.368779 11.00000 0.08181 AFIX 6 O53 4 0.880871 0.684755 0.131892 11.00000 0.18974 H53A 2 0.838386 0.679071 0.111219 11.00000 -1.50000 H53B 2 0.875517 0.692848 0.165885 11.00000 -1.50000 AFIX 0 O42 4 0.040911 0.638911 0.330612 11.00000 0.38608 0.06618 = 0.13847 0.04728 0.09474 0.05028 NA2 7 -0.358083 0.582218 0.322016 11.00000 0.16455 0.14618 = 0.07936 -0.01200 0.02425 0.06164 O49 4 -0.367329 0.616797 0.404530 11.00000 0.15152 AFIX 6 O57 4 0.632084 0.483915 0.232622 11.00000 0.16170 H57A 2 0.648272 0.506113 0.243234 11.00000 -1.50000 H57B 2 0.647105 0.477497 0.201069 11.00000 -1.50000 AFIX 0 O48 4 -0.337146 0.553115 0.229006 11.00000 0.21775 AFIX 6 O52 4 0.898361 0.929942 0.508317 11.00000 0.08317 H52A 2 0.889247 0.953677 0.509707 11.00000 -1.50000 H52B 2 0.861469 0.917315 0.515871 11.00000 -1.50000 AFIX 0 HKLF 4 REM CF solution in C2/c REM R1 = 0.0849 for 10879 Fo > 4sig(Fo) and 0.1233 for all 15635 data REM 864 parameters refined using 0 restraints END WGHT 0.1628 1134.5468 REM Instructions for potential hydrogen bonds HTAB O35 O39_$1 HTAB O33 O49_$2 HTAB O37 O52_$3 HTAB O39 O58_$4 HTAB O39 O53_$4 HTAB O29 O43_$5 HTAB C12 O19_$2 HTAB C19 O51_$5 HTAB O55 O5_$6 HTAB O55 O44_$6 HTAB C26 O41 HTAB O58 O39_$4 HTAB O56 O36_$6 HTAB O56 O56_$7 HTAB O54 O43 EQIV $12 -x, -y+1, -z+1 HTAB O54 O47_$12 HTAB O47 O37_$8 HTAB O53 O29_$9 HTAB O53 O43_$4 HTAB O53 O58 HTAB O57 O48_$6 HTAB O57 O2_$11 HTAB O52 O4_$5 HTAB O52 O49_$5 REM Highest difference peak 7.785, deepest hole -4.047, 1-sigma level 0.657 Q1 1 -0.1035 0.4963 0.7277 11.00000 0.05 7.78 Q2 1 -0.2217 0.6069 0.5787 11.00000 0.05 7.42 Q3 1 -0.0821 0.6699 0.6679 11.00000 0.05 7.42 Q4 1 0.0428 0.5787 0.5499 11.00000 0.05 7.15 Q5 1 -0.0787 0.4974 0.6626 11.00000 0.05 7.14 Q6 1 -0.0209 0.5789 0.6115 11.00000 0.05 7.13 Q7 1 0.2252 0.5804 0.6601 11.00000 0.05 6.80 Q8 1 -0.0969 0.6704 0.7249 11.00000 0.05 6.61 Q9 1 0.0622 0.7890 0.4135 11.00000 0.05 6.43 Q10 1 -0.3167 0.6118 0.6935 11.00000 0.05 6.40 Q11 1 -0.1536 0.6074 0.5185 11.00000 0.05 6.26 Q12 1 0.1598 0.5801 0.7205 11.00000 0.05 6.25 Q13 1 -0.2456 0.6122 0.6292 11.00000 0.05 6.06 Q14 1 -0.0050 0.6703 0.6036 11.00000 0.05 6.01 Q15 1 -0.1989 0.5270 0.5748 11.00000 0.05 5.97 Q16 1 -0.0082 0.4965 0.6008 11.00000 0.05 5.96 Q17 1 -0.2704 0.5264 0.6417 11.00000 0.05 5.83 Q18 1 -0.1763 0.6695 0.7867 11.00000 0.05 5.64 Q19 1 0.1786 0.4970 0.7092 11.00000 0.05 5.54 Q20 1 -0.0068 0.7898 0.4777 11.00000 0.05 5.51 ; _shelx_res_checksum 59840 loop_ _space_group_symop_operation_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' 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 W6 W 0.01293(5) 0.57936(2) 0.58028(4) 0.0248(2) Uani 1 1 d . . W5 W -0.04582(5) 0.67001(2) 0.63752(4) 0.0246(2) Uani 1 1 d . . W4 W -0.13497(5) 0.66988(2) 0.75371(4) 0.0257(2) Uani 1 1 d . . W8 W 0.19319(5) 0.57969(3) 0.68902(4) 0.0266(2) Uani 1 1 d . . W7 W -0.04182(6) 0.49699(2) 0.63239(4) 0.0274(2) Uani 1 1 d . . W1 W -0.18574(5) 0.60759(3) 0.54850(4) 0.0278(2) Uani 1 1 d . . W9 W 0.13918(5) 0.49705(3) 0.74098(4) 0.0283(2) Uani 1 1 d . . W2 W -0.28212(5) 0.61164(3) 0.66025(4) 0.0289(2) Uani 1 1 d . . W3 W -0.23783(5) 0.52611(3) 0.60865(4) 0.0307(2) Uani 1 1 d . . Yb1 Yb 0.02681(6) 0.78954(3) 0.44552(4) 0.0326(3) Uani 1 1 d . . P1 P -0.0944(3) 0.58212(13) 0.6930(2) 0.0146(10) Uani 1 1 d . . O17 O -0.0379(9) 0.5617(4) 0.6637(6) 0.027(3) Uani 1 1 d . . O23 O 0.2524(9) 0.5857(5) 0.6413(7) 0.033(4) Uiso 1 1 d . . O7 O -0.1705(10) 0.5815(4) 0.6467(6) 0.029(4) Uani 1 1 d . . O15 O 0.0437(10) 0.5865(4) 0.5160(9) 0.042(5) Uani 1 1 d . . O14 O 0.0064(8) 0.6290(4) 0.6090(6) 0.025(3) Uani 1 1 d . . O3 O -0.2705(10) 0.6245(5) 0.5829(7) 0.035(4) Uani 1 1 d . . O20 O 0.1029(10) 0.5717(4) 0.6304(7) 0.031(4) Uani 1 1 d . . O9 O -0.0974(8) 0.5867(4) 0.5453(7) 0.026(3) Uiso 1 1 d . . O25 O 0.2000(9) 0.5261(5) 0.6975(7) 0.031(4) Uani 1 1 d . . O36 O -0.0638(9) 0.7831(5) 0.3528(8) 0.036(4) Uani 1 1 d . . O40 O 0.0894(9) 0.7633(5) 0.3764(7) 0.033(4) Uani 1 1 d . . O10 O -0.1326(9) 0.6491(4) 0.5892(6) 0.024(3) Uani 1 1 d . . O35 O -0.1799(9) 0.7786(5) 0.3052(7) 0.033(4) Uani 1 1 d . . H35 H -0.1609 0.7772 0.2755 0.049 Uiso 1 1 calc R U O19 O -0.1023(8) 0.6953(4) 0.6892(6) 0.024(3) Uani 1 1 d . . O21 O 0.0586(9) 0.4979(4) 0.6787(7) 0.032(4) Uani 1 1 d . . O8 O -0.2196(9) 0.6499(4) 0.6960(7) 0.030(4) Uani 1 1 d . . O31 O -0.0011(14) 0.6660(6) 0.4666(12) 0.068(6) Uani 1 1 d . . O27 O 0.2123(9) 0.5088(5) 0.8123(8) 0.038(4) Uani 1 1 d . . O41 O 0.0390(11) 0.5480(5) 0.3956(7) 0.037(4) Uani 1 1 d . . O16 O -0.0077(9) 0.5251(4) 0.5739(7) 0.030(3) Uani 1 1 d . . O1 O -0.2943(9) 0.4907(5) 0.5758(8) 0.037(4) Uani 1 1 d . . O22 O 0.1557(9) 0.6293(4) 0.6987(6) 0.030(3) Uani 1 1 d . . O5 O -0.2094(10) 0.6250(5) 0.4784(7) 0.035(4) Uani 1 1 d . . O28 O 0.2604(9) 0.5874(5) 0.7622(8) 0.038(4) Uani 1 1 d . . O13 O 0.0415(8) 0.6761(4) 0.6981(6) 0.022(3) Uani 1 1 d . . N3 N 0.0586(12) 0.8349(7) 0.3731(9) 0.040(5) Uani 1 1 d . . O2 O -0.3103(9) 0.5604(5) 0.6297(7) 0.036(4) Uani 1 1 d . . O18 O -0.0735(8) 0.4880(4) 0.7067(6) 0.026(3) Uiso 1 1 d . . O26 O 0.1713(10) 0.4520(5) 0.7323(7) 0.039(4) Uani 1 1 d . . Na1 Na 0.0383(14) 0.6136(4) 0.4216(6) 0.113(8) Uani 1 1 d . . O33 O -0.0629(13) 0.8094(7) 0.6089(8) 0.063(6) Uani 1 1 d . . H33 H -0.1070 0.8144 0.6080 0.094 Uiso 1 1 calc R U O12 O -0.0317(10) 0.7069(4) 0.5932(6) 0.031(4) Uani 1 1 d . . O6 O -0.1418(9) 0.5096(5) 0.5983(7) 0.032(4) Uani 1 1 d . . O37 O -0.0159(13) 0.9149(5) 0.4307(10) 0.053(5) Uani 1 1 d . . H37 H -0.0364 0.9166 0.4596 0.080 Uiso 1 1 calc R U N2 N -0.1037(10) 0.7903(5) 0.4545(8) 0.028(4) Uani 1 1 d . . O32 O -0.0153(9) 0.7267(5) 0.4422(8) 0.038(4) Uani 1 1 d . . O34 O 0.0091(12) 0.7941(6) 0.5448(8) 0.047(5) Uani 1 1 d . . O38 O -0.0085(12) 0.8533(5) 0.4595(8) 0.044(5) Uani 1 1 d . . O39 O 0.1377(10) 0.7655(6) 0.2930(7) 0.041(4) Uani 1 1 d . . H39 H 0.1442 0.7427 0.3007 0.061 Uiso 1 1 calc R U N1 N 0.1117(10) 0.7449(5) 0.5052(8) 0.027(4) Uiso 1 1 d . . O4 O -0.2351(8) 0.5591(5) 0.5402(7) 0.029(3) Uani 1 1 d . . O30 O 0.1387(12) 0.8168(6) 0.4895(8) 0.050(5) Uani 1 1 d . . C9 C -0.1208(18) 0.7952(7) 0.5087(10) 0.041(7) Uani 1 1 d . . O29 O 0.2470(14) 0.8154(7) 0.5570(11) 0.073(7) Uani 1 1 d . . H29 H 0.2475 0.8380 0.5482 0.109 Uiso 1 1 calc R U C12 C -0.2342(15) 0.7867(7) 0.4120(13) 0.041(6) Uani 1 1 d . . H12 H -0.2725 0.7834 0.3791 0.049 Uiso 1 1 calc R U C10 C -0.1938(17) 0.7965(7) 0.5171(10) 0.038(6) Uani 1 1 d . . H10 H -0.2044 0.8001 0.5550 0.046 Uiso 1 1 calc R U C13 C -0.1574(18) 0.7865(6) 0.4065(13) 0.045(7) Uani 1 1 d . . C18 C 0.0917(16) 0.8847(9) 0.2882(12) 0.047(7) Uani 1 1 d . . H18 H 0.1026 0.9019 0.2600 0.057 Uiso 1 1 calc R U C6 C 0.0920(15) 0.7094(7) 0.5088(11) 0.039(6) Uani 1 1 d . . C2 C 0.1754(13) 0.7586(7) 0.5380(11) 0.035(5) Uani 1 1 d . . C5 C 0.1360(16) 0.6846(7) 0.5479(13) 0.045(7) Uani 1 1 d . . H5 H 0.1217 0.6593 0.5512 0.054 Uiso 1 1 calc R U C11 C -0.2491(19) 0.7923(8) 0.4692(13) 0.050(8) Uani 1 1 d . . H11 H -0.2984 0.7931 0.4743 0.060 Uiso 1 1 calc R U C4 C 0.2002(19) 0.6980(10) 0.5813(15) 0.060(9) Uani 1 1 d . . H4 H 0.2313 0.6818 0.6071 0.072 Uiso 1 1 calc R U C1 C 0.1874(19) 0.7999(8) 0.5283(13) 0.049(7) Uani 1 1 d . . C19 C 0.1091(15) 0.8475(9) 0.2857(11) 0.044(7) Uani 1 1 d . . H19 H 0.1331 0.8388 0.2558 0.052 Uiso 1 1 calc R U O11 O -0.0738(8) 0.6237(4) 0.7058(6) 0.024(3) Uani 1 1 d . . O24 O 0.1096(8) 0.5613(4) 0.7518(6) 0.020(3) Uani 1 1 d . . C21 C 0.1083(12) 0.7810(7) 0.3320(10) 0.030(5) Uani 1 1 d . . C8 C -0.0547(17) 0.7978(9) 0.5583(12) 0.048(7) Uani 1 1 d . . C7 C 0.0215(15) 0.6995(8) 0.4694(13) 0.044(7) Uani 1 1 d . . C20 C 0.0910(14) 0.8216(6) 0.3282(11) 0.034(6) Uani 1 1 d . . C14 C -0.1287(16) 0.7838(7) 0.3515(13) 0.040(6) Uani 1 1 d . . C15 C 0.0040(16) 0.8801(8) 0.4249(12) 0.042(6) Uani 1 1 d . . C3 C 0.2197(16) 0.7358(9) 0.5771(11) 0.044(7) Uani 1 1 d . . H3 H 0.2629 0.7454 0.6010 0.053 Uiso 1 1 calc R U C17 C 0.0570(16) 0.8969(8) 0.3341(15) 0.052(8) Uani 1 1 d . . H17 H 0.0440 0.9225 0.3362 0.063 Uiso 1 1 calc R U C16 C 0.0414(17) 0.8719(7) 0.3763(13) 0.044(6) Uani 1 1 d . . O43 O 0.172(2) 0.6123(13) 0.440(2) 0.152(17) Uani 1 1 d . . O44 O -0.105(2) 0.6078(11) 0.382(2) 0.138(15) Uani 1 1 d . . O50 O 0.1812(10) 0.7070(5) 0.7204(8) 0.036(4) Uani 1 1 d . . O51 O 0.3671(8) 0.6298(5) 0.8382(7) 0.037(4) Uani 1 1 d . . C22 C -0.350(4) 0.496(2) 0.400(3) 0.14(2) Uiso 1 1 d . . O55 O 0.842(2) 0.6921(12) 0.4185(18) 0.120(12) Uani 1 1 d G . H55A H 0.8569 0.6691 0.4191 0.181 Uiso 1 1 d G U H55B H 0.8395 0.7013 0.3837 0.181 Uiso 1 1 d G U C26 C -0.131(2) 0.5339(11) 0.4336(17) 0.071(10) Uiso 1 1 d . . H26 H -0.0823 0.5426 0.4392 0.085 Uiso 1 1 calc R U O58 O 0.832(3) 0.6944(16) 0.2311(14) 0.16(2) Uani 1 1 d G . H58A H 0.8401 0.7128 0.2088 0.238 Uiso 1 1 d G U H58B H 0.8237 0.6741 0.2103 0.238 Uiso 1 1 d G U C24 C -0.221(2) 0.4887(11) 0.4479(16) 0.063(9) Uiso 1 1 d . . H24 H -0.2350 0.4660 0.4635 0.076 Uiso 1 1 calc R U O45 O -0.232(2) 0.6092(10) 0.3384(15) 0.125(14) Uani 1 1 d . . O56 O 0.958(3) 0.7051(10) 0.2968(16) 0.114(12) Uani 1 1 d G . H56A H 0.9407 0.7136 0.3260 0.170 Uiso 1 1 d G U H56B H 0.9933 0.7197 0.2904 0.170 Uiso 1 1 d G U C25 C -0.144(2) 0.5027(10) 0.4593(16) 0.062(9) Uiso 1 1 d . . H25 H -0.1057 0.4895 0.4840 0.074 Uiso 1 1 calc R U N4 N -0.258(2) 0.5427(11) 0.3871(16) 0.083(10) Uiso 1 1 d . . O54 O 0.331(7) 0.593(4) 0.509(5) 0.80(15) Uani 1 1 d G . H54A H 0.2855 0.5875 0.5088 1.194 Uiso 1 1 d G U H54B H 0.3587 0.5795 0.5357 1.194 Uiso 1 1 d G U C23 C -0.269(2) 0.5116(12) 0.4131(18) 0.076(10) Uiso 1 1 d . . O47 O -0.368(3) 0.4720(16) 0.4345(19) 0.16(2) Uani 1 1 d . . H47 H -0.4117 0.4661 0.4233 0.245 Uiso 1 1 calc R U O46 O -0.4010(12) 0.5198(8) 0.3635(10) 0.071(7) Uani 1 1 d . . C27 C -0.185(2) 0.5555(12) 0.3984(18) 0.078(11) Uiso 1 1 d . . C28 C -0.172(3) 0.5933(14) 0.369(2) 0.082(11) Uiso 1 1 d . . O53 O 0.881(4) 0.685(2) 0.132(2) 0.19(2) Uiso 1 1 d G . H53A H 0.8384 0.6791 0.1112 0.285 Uiso 1 1 d G U H53B H 0.8755 0.6928 0.1659 0.285 Uiso 1 1 d G U O42 O 0.041(4) 0.6389(10) 0.3306(19) 0.19(3) Uani 1 1 d . . Na2 Na -0.3581(15) 0.5822(7) 0.3220(9) 0.130(9) Uani 1 1 d . . O49 O -0.367(3) 0.6168(13) 0.405(2) 0.152(16) Uiso 1 1 d . . O57 O 0.632(3) 0.4839(19) 0.233(2) 0.162(17) Uiso 1 1 d G . H57A H 0.6483 0.5061 0.2432 0.243 Uiso 1 1 d G U H57B H 0.6471 0.4775 0.2011 0.243 Uiso 1 1 d G U O48 O -0.337(4) 0.5531(19) 0.229(3) 0.22(2) Uiso 1 1 d . . O52 O 0.8984(16) 0.9299(9) 0.5083(14) 0.083(8) Uiso 1 1 d G . H52A H 0.8892 0.9537 0.5097 0.125 Uiso 1 1 d G U H52B H 0.8615 0.9173 0.5159 0.125 Uiso 1 1 d G 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 W6 0.0310(5) 0.0247(4) 0.0210(4) -0.0015(3) 0.0108(4) 0.0012(3) W5 0.0343(5) 0.0194(4) 0.0218(4) 0.0019(3) 0.0097(4) 0.0011(3) W4 0.0328(5) 0.0221(4) 0.0242(4) -0.0021(3) 0.0106(4) 0.0043(3) W8 0.0277(5) 0.0308(5) 0.0237(4) -0.0017(3) 0.0110(4) 0.0002(3) W7 0.0376(5) 0.0198(4) 0.0260(4) -0.0045(3) 0.0088(4) 0.0008(3) W1 0.0323(5) 0.0283(5) 0.0232(4) -0.0003(3) 0.0065(4) 0.0034(4) W9 0.0357(5) 0.0221(4) 0.0281(5) -0.0019(3) 0.0087(4) 0.0050(3) W2 0.0289(5) 0.0330(5) 0.0259(4) -0.0014(4) 0.0077(4) 0.0039(4) W3 0.0342(5) 0.0291(5) 0.0281(5) -0.0027(4) 0.0039(4) -0.0032(4) Yb1 0.0393(6) 0.0324(6) 0.0277(5) 0.0033(4) 0.0101(4) 0.0041(4) P1 0.028(3) 0.005(2) 0.014(2) 0.0004(16) 0.012(2) -0.0006(17) O17 0.043(9) 0.014(7) 0.024(7) 0.008(6) 0.010(7) 0.003(6) O7 0.050(10) 0.016(7) 0.020(7) 0.011(6) 0.006(7) 0.002(6) O15 0.047(11) 0.021(8) 0.070(13) -0.025(8) 0.040(10) -0.009(7) O14 0.028(8) 0.032(8) 0.016(7) -0.004(6) 0.004(6) -0.001(6) O3 0.047(10) 0.038(9) 0.020(7) -0.011(7) 0.008(7) -0.010(8) O20 0.049(10) 0.022(8) 0.029(8) -0.002(6) 0.025(8) 0.004(7) O25 0.033(9) 0.034(9) 0.032(8) -0.005(7) 0.021(7) 0.003(7) O36 0.024(8) 0.046(10) 0.035(9) 0.007(8) 0.001(7) 0.010(7) O40 0.040(9) 0.036(9) 0.023(8) -0.006(7) 0.003(7) -0.005(7) O10 0.033(8) 0.020(7) 0.019(7) -0.004(6) 0.004(6) -0.001(6) O35 0.036(9) 0.034(9) 0.026(8) 0.008(7) -0.001(7) 0.001(7) O19 0.035(8) 0.016(7) 0.020(7) 0.005(5) 0.003(6) -0.002(6) O21 0.037(9) 0.024(8) 0.035(9) -0.005(7) 0.010(8) 0.006(7) O8 0.040(9) 0.027(8) 0.029(8) -0.010(6) 0.019(7) -0.003(7) O31 0.067(15) 0.049(13) 0.088(18) 0.006(12) 0.015(14) -0.012(11) O27 0.036(9) 0.029(9) 0.053(11) 0.008(8) 0.023(9) 0.007(7) O41 0.061(12) 0.024(8) 0.027(8) -0.007(7) 0.011(8) 0.004(8) O16 0.038(9) 0.026(8) 0.028(8) 0.001(6) 0.011(7) 0.009(7) O1 0.033(9) 0.042(10) 0.036(9) -0.010(8) 0.004(8) -0.017(8) O22 0.045(9) 0.030(8) 0.011(6) -0.008(6) 0.000(6) -0.010(7) O5 0.050(11) 0.026(8) 0.029(8) 0.007(7) 0.008(8) 0.010(7) O28 0.030(9) 0.053(11) 0.035(9) 0.003(8) 0.018(8) 0.013(8) O13 0.028(8) 0.018(7) 0.022(7) 0.003(5) 0.006(6) -0.001(6) N3 0.036(12) 0.046(13) 0.036(11) 0.006(10) 0.002(10) 0.003(10) O2 0.033(9) 0.037(9) 0.037(9) 0.002(7) 0.005(8) -0.004(7) O26 0.047(10) 0.035(10) 0.031(9) 0.003(7) 0.003(8) 0.021(8) Na1 0.25(3) 0.044(8) 0.041(7) -0.006(6) 0.017(11) 0.008(11) O33 0.067(14) 0.096(18) 0.033(10) 0.006(11) 0.029(10) 0.013(13) O12 0.062(11) 0.017(7) 0.017(7) 0.004(6) 0.015(7) -0.004(7) O6 0.039(9) 0.031(8) 0.022(7) -0.001(6) -0.006(7) 0.002(7) O37 0.074(15) 0.036(11) 0.059(13) 0.001(9) 0.035(12) -0.002(10) N2 0.027(10) 0.033(10) 0.024(9) -0.003(8) 0.006(8) 0.007(8) O32 0.035(9) 0.038(10) 0.037(9) -0.008(8) 0.000(8) -0.009(7) O34 0.067(13) 0.049(11) 0.028(9) 0.006(8) 0.015(9) 0.013(10) O38 0.067(13) 0.026(9) 0.044(10) 0.000(8) 0.021(10) 0.005(8) O39 0.042(10) 0.052(11) 0.031(9) -0.002(8) 0.016(8) 0.010(9) O4 0.023(8) 0.038(9) 0.027(8) -0.011(7) 0.003(6) 0.003(7) O30 0.063(13) 0.048(12) 0.035(10) -0.009(9) 0.001(9) -0.013(10) C9 0.08(2) 0.031(13) 0.021(11) -0.005(9) 0.018(13) -0.017(13) O29 0.081(17) 0.051(14) 0.076(16) 0.010(12) -0.011(14) -0.033(12) C12 0.038(14) 0.036(14) 0.046(15) 0.014(12) 0.005(12) 0.009(11) C10 0.07(2) 0.021(11) 0.019(11) 0.008(9) 0.007(12) 0.006(11) C13 0.07(2) 0.011(10) 0.057(17) 0.001(10) 0.026(16) -0.001(11) C18 0.048(16) 0.055(18) 0.041(15) 0.030(13) 0.015(13) 0.015(13) C6 0.046(15) 0.039(14) 0.037(13) -0.001(11) 0.021(12) 0.007(11) C2 0.026(11) 0.038(14) 0.034(12) 0.007(11) -0.008(10) 0.003(10) C5 0.052(17) 0.026(13) 0.063(18) 0.016(12) 0.025(15) 0.006(11) C11 0.07(2) 0.035(14) 0.056(18) 0.019(13) 0.050(17) 0.016(13) C4 0.053(19) 0.07(2) 0.06(2) 0.030(17) 0.018(17) 0.016(16) C1 0.07(2) 0.037(15) 0.038(15) -0.004(12) 0.005(15) 0.005(14) C19 0.038(14) 0.059(18) 0.030(12) 0.016(12) -0.005(11) -0.012(13) O11 0.033(8) 0.021(7) 0.022(7) -0.002(6) 0.015(6) -0.003(6) O24 0.019(7) 0.029(8) 0.010(6) -0.010(5) 0.001(5) 0.000(6) C21 0.019(10) 0.042(13) 0.024(10) 0.006(10) -0.008(9) 0.013(9) C8 0.059(18) 0.052(17) 0.041(15) 0.002(13) 0.028(14) 0.022(14) C7 0.039(14) 0.042(15) 0.053(17) 0.021(13) 0.015(13) 0.007(12) C20 0.045(14) 0.024(11) 0.037(13) 0.009(10) 0.017(11) 0.022(10) C14 0.052(17) 0.022(12) 0.049(15) 0.009(11) 0.021(14) 0.002(11) C15 0.047(15) 0.039(14) 0.038(14) 0.022(12) 0.005(12) 0.022(12) C3 0.047(16) 0.059(18) 0.032(13) 0.003(12) 0.020(12) 0.008(13) C17 0.041(16) 0.039(15) 0.08(2) 0.000(15) 0.027(16) -0.010(12) C16 0.061(18) 0.016(11) 0.050(16) -0.001(10) 0.003(14) -0.003(11) O43 0.14(3) 0.15(4) 0.18(4) 0.03(3) 0.06(3) -0.06(3) O44 0.16(4) 0.10(3) 0.18(4) -0.02(3) 0.08(3) -0.03(3) O50 0.044(10) 0.025(8) 0.042(9) 0.006(7) 0.017(8) -0.011(7) O51 0.018(7) 0.060(12) 0.032(9) -0.018(8) 0.000(7) -0.003(7) O55 0.061(19) 0.14(3) 0.17(4) 0.02(3) 0.04(2) 0.00(2) O58 0.21(5) 0.22(5) 0.052(17) 0.04(3) 0.03(2) -0.08(4) O45 0.17(4) 0.11(3) 0.09(2) 0.01(2) 0.01(2) 0.06(3) O56 0.14(3) 0.09(2) 0.10(2) -0.038(19) 0.01(3) 0.02(2) O54 0.72(19) 0.9(2) 0.53(14) 0.69(17) -0.40(14) -0.40(17) O47 0.14(4) 0.25(6) 0.10(3) 0.00(3) 0.02(3) -0.07(4) O46 0.040(12) 0.11(2) 0.059(14) 0.004(14) 0.000(11) 0.016(13) O42 0.39(8) 0.07(2) 0.14(3) 0.05(2) 0.09(4) 0.05(3) Na2 0.16(2) 0.15(2) 0.079(13) -0.012(12) 0.024(14) 0.062(16) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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' Yb Yb -0.3850 5.5486 '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 O15 W6 O20 99.1(8) . . O15 W6 O14 102.8(7) . . O20 W6 O14 91.6(7) . . O15 W6 O16 99.9(7) . . O20 W6 O16 92.3(7) . . O14 W6 O16 156.1(6) . . O15 W6 O9 96.2(8) . . O20 W6 O9 164.7(6) . . O14 W6 O9 84.0(6) . . O16 W6 O9 86.0(6) . . O15 W6 O17 172.1(7) . . O20 W6 O17 84.3(6) . . O14 W6 O17 84.2(6) . . O16 W6 O17 72.7(6) . . O9 W6 O17 80.7(6) . . O12 W5 O10 98.8(7) . . O12 W5 O14 103.1(7) . . O10 W5 O14 85.8(6) . . O12 W5 O13 98.4(7) . . O10 W5 O13 162.2(6) . . O14 W5 O13 86.0(6) . . O12 W5 O19 100.2(7) . . O10 W5 O19 92.8(6) . . O14 W5 O19 156.6(6) . . O13 W5 O19 88.5(6) . . O12 W5 O11 172.9(6) . . O10 W5 O11 81.8(6) . . O14 W5 O11 84.0(6) . . O13 W5 O11 81.7(6) . . O19 W5 O11 72.7(5) . . O50 W4 O13 99.3(8) 2_556 2_556 O50 W4 O22 102.0(7) 2_556 2_556 O13 W4 O22 90.6(7) 2_556 2_556 O50 W4 O19 99.2(7) 2_556 . O13 W4 O19 90.9(6) 2_556 . O22 W4 O19 158.2(6) 2_556 . O50 W4 O8 97.3(8) 2_556 . O13 W4 O8 163.3(6) 2_556 . O22 W4 O8 84.1(7) 2_556 . O19 W4 O8 88.3(6) . . O50 W4 O11 172.1(7) 2_556 . O13 W4 O11 83.9(6) 2_556 . O22 W4 O11 85.1(6) 2_556 . O19 W4 O11 73.4(5) . . O8 W4 O11 79.9(6) . . O23 W8 O25 98.8(7) . . O23 W8 O28 99.6(8) . . O25 W8 O28 91.9(8) . . O23 W8 O22 104.5(7) . . O25 W8 O22 156.5(6) . . O28 W8 O22 87.3(7) . . O23 W8 O20 97.8(7) . . O25 W8 O20 87.6(7) . . O28 W8 O20 162.5(6) . . O22 W8 O20 86.3(6) . . O23 W8 O24 171.3(6) . . O25 W8 O24 72.9(5) . . O28 W8 O24 83.6(6) . . O22 W8 O24 83.7(6) . . O20 W8 O24 79.5(5) . . O41 W7 O16 100.4(7) 5_566 . O41 W7 O6 99.1(8) 5_566 . O16 W7 O6 90.6(7) . . O41 W7 O18 102.5(7) 5_566 . O16 W7 O18 157.0(6) . . O6 W7 O18 88.4(7) . . O41 W7 O21 97.3(8) 5_566 . O16 W7 O21 88.4(7) . . O6 W7 O21 163.5(6) . . O18 W7 O21 86.1(7) . . O41 W7 O17 173.7(7) 5_566 . O16 W7 O17 73.5(6) . . O6 W7 O17 82.6(6) . . O18 W7 O17 83.6(6) . . O21 W7 O17 81.3(6) . . O5 W1 O9 100.2(8) . . O5 W1 O10 101.6(7) . . O9 W1 O10 87.4(7) . . O5 W1 O4 101.4(8) . . O9 W1 O4 92.5(7) . . O10 W1 O4 156.6(6) . . O5 W1 O3 101.1(8) . . O9 W1 O3 158.6(7) . . O10 W1 O3 86.5(6) . . O4 W1 O3 85.1(7) . . O5 W1 O7 172.0(8) . . O9 W1 O7 86.4(6) . . O10 W1 O7 82.9(6) . . O4 W1 O7 73.8(6) . . O3 W1 O7 72.4(6) . . O26 W9 O21 99.5(8) . . O26 W9 O18 101.1(8) . 2_556 O21 W9 O18 89.0(7) . 2_556 O26 W9 O25 100.7(8) . . O21 W9 O25 92.7(7) . . O18 W9 O25 157.5(6) 2_556 . O26 W9 O27 95.7(8) . . O21 W9 O27 164.6(7) . . O18 W9 O27 85.4(7) 2_556 . O25 W9 O27 87.1(7) . . O26 W9 O24 173.1(7) . . O21 W9 O24 84.3(6) . . O18 W9 O24 84.7(6) 2_556 . O25 W9 O24 73.2(6) . . O27 W9 O24 80.9(6) . . O51 W2 O8 102.1(8) 2_556 . O51 W2 O3 101.5(8) 2_556 . O8 W2 O3 94.1(7) . . O51 W2 O28 100.1(7) 2_556 2_556 O8 W2 O28 85.0(7) . 2_556 O3 W2 O28 158.1(8) . 2_556 O51 W2 O2 100.1(8) 2_556 . O8 W2 O2 157.1(7) . . O3 W2 O2 87.3(7) . . O28 W2 O2 85.3(7) 2_556 . O51 W2 O7 172.3(7) 2_556 . O8 W2 O7 84.8(6) . . O3 W2 O7 74.2(7) . . O28 W2 O7 83.9(6) 2_556 . O2 W2 O7 73.6(6) . . O1 W3 O27 102.0(8) . 2_556 O1 W3 O6 102.6(8) . . O27 W3 O6 87.5(7) 2_556 . O1 W3 O2 100.4(8) . . O27 W3 O2 91.0(7) 2_556 . O6 W3 O2 156.7(7) . . O1 W3 O4 100.7(8) . . O27 W3 O4 157.2(7) 2_556 . O6 W3 O4 85.1(6) . . O2 W3 O4 87.4(7) . . O1 W3 O7 172.1(7) . . O27 W3 O7 84.0(6) 2_556 . O6 W3 O7 82.5(6) . . O2 W3 O7 74.2(6) . . O4 W3 O7 73.6(6) . . O30 Yb1 O40 87.1(6) . . O30 Yb1 O32 131.7(7) . . O40 Yb1 O32 78.7(6) . . O30 Yb1 O34 80.0(7) . . O40 Yb1 O34 149.5(6) . . O32 Yb1 O34 89.4(7) . . O30 Yb1 O38 77.9(7) . . O40 Yb1 O38 130.7(6) . . O32 Yb1 O38 143.3(7) . . O34 Yb1 O38 73.4(6) . . O30 Yb1 N1 66.8(7) . . O40 Yb1 N1 77.4(6) . . O32 Yb1 N1 65.1(6) . . O34 Yb1 N1 72.2(6) . . O38 Yb1 N1 134.0(7) . . O30 Yb1 N2 139.4(7) . . O40 Yb1 N2 133.1(6) . . O32 Yb1 N2 72.0(6) . . O34 Yb1 N2 66.4(7) . . O38 Yb1 N2 71.4(7) . . N1 Yb1 N2 119.3(6) . . O30 Yb1 O36 144.6(6) . . O40 Yb1 O36 73.2(6) . . O32 Yb1 O36 73.7(6) . . O34 Yb1 O36 130.4(7) . . O38 Yb1 O36 92.7(6) . . N1 Yb1 O36 133.0(6) . . N2 Yb1 O36 64.0(6) . . O30 Yb1 N3 73.7(7) . . O40 Yb1 N3 65.4(7) . . O32 Yb1 N3 135.5(7) . . O34 Yb1 N3 134.6(7) . . O38 Yb1 N3 65.3(7) . . N1 Yb1 N3 126.2(7) . . N2 Yb1 N3 114.5(7) . . O36 Yb1 N3 71.4(7) . . O30 Yb1 C1 19.4(7) . . O40 Yb1 C1 86.1(7) . . O32 Yb1 C1 112.8(7) . . O34 Yb1 C1 72.7(8) . . O38 Yb1 C1 93.1(7) . . N1 Yb1 C1 47.6(7) . . N2 Yb1 C1 138.8(7) . . O36 Yb1 C1 156.9(7) . . N3 Yb1 C1 90.9(8) . . O30 Yb1 C7 112.8(7) . . O40 Yb1 C7 76.1(6) . . O32 Yb1 C7 19.0(7) . . O34 Yb1 C7 83.6(7) . . O38 Yb1 C7 152.8(7) . . N1 Yb1 C7 46.2(7) . . N2 Yb1 C7 86.3(7) . . O36 Yb1 C7 91.1(7) . . N3 Yb1 C7 140.7(7) . . C1 Yb1 C7 93.8(7) . . O17 P1 O11 112.0(8) . . O17 P1 O24 112.9(8) . 2_556 O11 P1 O24 112.0(8) . 2_556 O17 P1 O7 106.5(9) . . O11 P1 O7 107.2(8) . . O24 P1 O7 105.7(8) 2_556 . P1 O17 W6 129.9(8) . . P1 O17 W7 126.9(9) . . W6 O17 W7 90.1(5) . . P1 O7 W2 125.1(8) . . P1 O7 W3 125.8(8) . . W2 O7 W3 90.9(6) . . P1 O7 W1 123.6(9) . . W2 O7 W1 90.2(5) . . W3 O7 W1 90.6(5) . . W6 O15 Na1 154.0(12) . . W6 O14 W5 152.9(9) . . W2 O3 W1 123.1(10) . . W6 O20 W8 162.5(9) . . W1 O9 W6 150.3(9) . . W8 O25 W9 123.3(7) . . C14 O36 Yb1 122.0(18) . . C21 O40 Yb1 126.0(15) . . W1 O10 W5 151.1(9) . . C14 O35 H35 109.5 . . W4 O19 W5 122.8(7) . . W9 O21 W7 163.1(10) . . W2 O8 W4 154.0(10) . . C7 O31 Na1 131(2) . . W3 O27 W9 151.6(9) 2_556 . W7 O41 Na1 172.0(10) 5_566 . W7 O16 W6 123.5(8) . . W4 O22 W8 151.8(8) 2_556 . W8 O28 W2 148.7(9) . 2_556 W4 O13 W5 163.6(9) 2_556 . C16 N3 C20 121(2) . . C16 N3 Yb1 120.3(18) . . C20 N3 Yb1 118.7(16) . . W3 O2 W2 121.3(9) . . W9 O18 W7 150.8(9) 2_556 . O42 Na1 O31 99.3(13) . . O42 Na1 O15 176(2) . . O31 Na1 O15 82.7(9) . . O42 Na1 O41 98.5(12) . . O31 Na1 O41 155.0(13) . . O15 Na1 O41 80.5(7) . . O42 Na1 O43 88(2) . . O31 Na1 O43 109.5(15) . . O15 Na1 O43 88.2(13) . . O41 Na1 O43 88.4(14) . . O42 Na1 O44 85(2) . . O31 Na1 O44 80.6(13) . . O15 Na1 O44 98.5(13) . . O41 Na1 O44 83.7(12) . . O43 Na1 O44 168.6(16) . . C8 O33 H33 109.4 . . W7 O6 W3 149.1(9) . . C15 O37 H37 109.5 . . C13 N2 C9 120(2) . . C13 N2 Yb1 120.5(16) . . C9 N2 Yb1 119.0(18) . . C7 O32 Yb1 123.9(17) . . C8 O34 Yb1 123.0(18) . . C15 O38 Yb1 121.8(16) . . C21 O39 H39 109.5 . . C6 N1 C2 122(2) . . C6 N1 Yb1 119.8(17) . . C2 N1 Yb1 118.2(15) . . W1 O4 W3 122.0(8) . . C1 O30 Yb1 123.6(19) . . N2 C9 C10 122(3) . . N2 C9 C8 114(2) . . C10 C9 C8 124(2) . . C1 O29 H29 109.5 . . C11 C12 C13 117(3) . . C11 C12 H12 121.6 . . C13 C12 H12 121.6 . . C11 C10 C9 118(2) . . C11 C10 H10 120.8 . . C9 C10 H10 120.8 . . N2 C13 C12 120(2) . . N2 C13 C14 113(3) . . C12 C13 C14 127(3) . . C19 C18 C17 118(3) . . C19 C18 H18 120.9 . . C17 C18 H18 120.8 . . N1 C6 C5 120(3) . . N1 C6 C7 114(2) . . C5 C6 C7 125(3) . . N1 C2 C3 120(3) . . N1 C2 C1 114(2) . . C3 C2 C1 126(3) . . C4 C5 C6 118(3) . . C4 C5 H5 120.9 . . C6 C5 H5 120.7 . . C10 C11 C12 122(3) . . C10 C11 H11 119.1 . . C12 C11 H11 119.2 . . C5 C4 C3 120(3) . . C5 C4 H4 119.9 . . C3 C4 H4 120.0 . . O29 C1 O30 125(3) . . O29 C1 C2 118(3) . . O30 C1 C2 117(3) . . O29 C1 Yb1 161(2) . . O30 C1 Yb1 37.0(14) . . C2 C1 Yb1 80.4(16) . . C18 C19 C20 120(3) . . C18 C19 H19 119.8 . . C20 C19 H19 119.9 . . P1 O11 W4 128.9(8) . . P1 O11 W5 127.3(8) . . W4 O11 W5 91.0(5) . . P1 O24 W9 128.9(8) 2_556 . P1 O24 W8 127.5(8) 2_556 . W9 O24 W8 90.5(4) . . O39 C21 O40 125(2) . . O39 C21 C20 120(2) . . O40 C21 C20 115(2) . . O33 C8 O34 122(3) . . O33 C8 C9 120(3) . . O34 C8 C9 117(2) . . O31 C7 O32 123(3) . . O31 C7 C6 120(3) . . O32 C7 C6 117(3) . . O31 C7 Yb1 160(2) . . O32 C7 Yb1 37.1(12) . . C6 C7 Yb1 79.6(15) . . N3 C20 C19 119(2) . . N3 C20 C21 114(2) . . C19 C20 C21 126(2) . . O36 C14 O35 126(2) . . O36 C14 C13 120(3) . . O35 C14 C13 113(2) . . O38 C15 O37 123(2) . . O38 C15 C16 120(2) . . O37 C15 C16 117(2) . . C2 C3 C4 119(3) . . C2 C3 H3 120.5 . . C4 C3 H3 120.5 . . C16 C17 C18 121(3) . . C16 C17 H17 119.3 . . C18 C17 H17 119.4 . . N3 C16 C17 120(3) . . N3 C16 C15 113(2) . . C17 C16 C15 127(2) . . C28 O44 Na1 161(4) . . O47 C22 O46 124(7) . . O47 C22 C23 118(7) . . O46 C22 C23 114(6) . . H55A O55 H55B 109.5 . . C25 C26 C27 125(4) . . C25 C26 H26 117.7 . . C27 C26 H26 117.7 . . H58A O58 H58B 109.5 . . C23 C24 C25 114(4) . . C23 C24 H24 123.2 . . C25 C24 H24 123.1 . . C28 O45 Na2 126(3) . . H56A O56 H56B 109.5 . . C26 C25 C24 117(4) . . C26 C25 H25 121.6 . . C24 C25 H25 121.5 . . C23 N4 C27 115(4) . . C23 N4 Na2 125(3) . . C27 N4 Na2 120(3) . . H54A O54 H54B 109.5 . . N4 C23 C24 131(4) . . N4 C23 C22 116(5) . . C24 C23 C22 113(5) . . C22 O47 H47 109.1 . . C22 O46 Na2 121(4) . . C26 C27 N4 119(4) . . C26 C27 C28 126(4) . . N4 C27 C28 115(4) . . O44 C28 O45 128(5) . . O44 C28 C27 117(4) . . O45 C28 C27 115(4) . . H53A O53 H53B 109.5 . . O49 Na2 O48 171(2) . . O49 Na2 O45 83.4(17) . . O48 Na2 O45 89.7(18) . . O49 Na2 N4 88.0(16) . . O48 Na2 N4 93.8(18) . . O45 Na2 N4 64.5(13) . . O49 Na2 O46 94.1(15) . . O48 Na2 O46 94.3(18) . . O45 Na2 O46 128.0(13) . . N4 Na2 O46 63.6(11) . . H57A O57 H57B 109.5 . . H52A O52 H52B 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 W6 O15 1.688(18) . W6 O20 1.832(18) . W6 O14 1.871(15) . W6 O16 1.940(16) . W6 O9 2.033(15) . W6 O17 2.355(14) . W5 O12 1.692(14) . W5 O10 1.894(15) . W5 O14 1.906(15) . W5 O13 1.912(15) . W5 O19 1.924(14) . W5 O11 2.372(14) . W4 O50 1.716(15) 2_556 W4 O13 1.856(15) 2_556 W4 O22 1.874(15) 2_556 W4 O19 1.912(13) . W4 O8 1.957(16) . W4 O11 2.351(14) . W8 O23 1.690(16) . W8 O25 1.889(16) . W8 O28 1.892(18) . W8 O22 1.894(16) . W8 O20 1.933(18) . W8 O24 2.373(13) . W7 O41 1.706(15) 5_566 W7 O16 1.860(15) . W7 O6 1.893(16) . W7 O18 1.920(14) . W7 O21 1.931(17) . W7 O17 2.375(14) . W1 O5 1.690(16) . W1 O9 1.785(15) . W1 O10 1.891(14) . W1 O4 1.916(16) . W1 O3 1.956(17) . W1 O7 2.388(14) . W9 O26 1.709(16) . W9 O21 1.839(17) . W9 O18 1.876(14) 2_556 W9 O25 1.917(15) . W9 O27 1.941(19) . W9 O24 2.340(14) . W2 O51 1.683(16) 2_556 W2 O8 1.845(16) . W2 O3 1.875(15) . W2 O28 1.937(18) 2_556 W2 O2 1.958(17) . W2 O7 2.367(17) . W3 O1 1.693(16) . W3 O27 1.877(19) 2_556 W3 O6 1.901(17) . W3 O2 1.914(17) . W3 O4 1.951(16) . W3 O7 2.369(16) . Yb1 O30 2.30(2) . Yb1 O40 2.310(16) . Yb1 O32 2.330(17) . Yb1 O34 2.356(17) . Yb1 O38 2.363(17) . Yb1 N1 2.427(19) . Yb1 N2 2.428(18) . Yb1 O36 2.435(17) . Yb1 N3 2.44(2) . Yb1 C1 3.19(3) . Yb1 C7 3.21(3) . P1 O17 1.512(15) . P1 O11 1.520(15) . P1 O24 1.529(13) 2_556 P1 O7 1.576(18) . O15 Na1 2.34(2) . O36 C14 1.18(3) . O40 C21 1.29(3) . O35 C14 1.28(3) . O35 H35 0.8200 . O31 C7 1.24(3) . O31 Na1 2.29(3) . O27 W3 1.877(19) 2_556 O41 W7 1.706(15) 5_566 O41 Na1 2.38(2) . O22 W4 1.874(15) 2_556 O28 W2 1.937(18) 2_556 O13 W4 1.855(14) 2_556 N3 C16 1.34(3) . N3 C20 1.36(3) . O18 W9 1.876(14) 2_556 Na1 O42 2.27(4) . Na1 O43 2.40(5) . Na1 O44 2.61(5) . O33 C8 1.26(3) . O33 H33 0.8200 . O37 C15 1.29(3) . O37 H37 0.8200 . N2 C13 1.33(4) . N2 C9 1.34(3) . O32 C7 1.26(3) . O34 C8 1.27(3) . O38 C15 1.28(3) . O39 C21 1.25(3) . O39 H39 0.8200 . N1 C6 1.30(3) . N1 C2 1.34(3) . O30 C1 1.27(4) . C9 C10 1.38(4) . C9 C8 1.49(4) . O29 C1 1.28(4) . O29 H29 0.8200 . C12 C11 1.40(4) . C12 C13 1.43(4) . C12 H12 0.9300 . C10 C11 1.35(4) . C10 H10 0.9300 . C13 C14 1.45(4) . C18 C19 1.35(4) . C18 C17 1.39(4) . C18 H18 0.9300 . C6 C5 1.39(4) . C6 C7 1.46(4) . C2 C3 1.35(4) . C2 C1 1.49(4) . C5 C4 1.35(5) . C5 H5 0.9300 . C11 H11 0.9300 . C4 C3 1.38(4) . C4 H4 0.9300 . C19 C20 1.41(3) . C19 H19 0.9300 . O24 P1 1.529(13) 2_556 C21 C20 1.46(3) . C15 C16 1.44(4) . C3 H3 0.9300 . C17 C16 1.37(4) . C17 H17 0.9300 . O44 C28 1.30(6) . O50 W4 1.716(15) 2_556 O51 W2 1.683(16) 2_556 C22 O47 1.24(8) . C22 O46 1.40(8) . C22 C23 1.55(8) . O55 H55A 0.8497 . O55 H55B 0.8503 . C26 C25 1.28(5) . C26 C27 1.37(5) . C26 H26 0.9300 . O58 H58A 0.8500 . O58 H58B 0.8499 . C24 C23 1.33(5) . C24 C25 1.46(5) . C24 H24 0.9300 . O45 C28 1.30(5) . O45 Na2 2.45(6) . O56 H56A 0.8501 . O56 H56B 0.8501 . C25 H25 0.9300 . N4 C23 1.27(5) . N4 C27 1.37(5) . N4 Na2 2.54(4) . O54 H54A 0.8498 . O54 H54B 0.8499 . O47 H47 0.8200 . O46 Na2 2.57(4) . C27 C28 1.53(6) . O53 H53A 0.8501 . O53 H53B 0.8498 . Na2 O49 2.27(5) . Na2 O48 2.45(7) . O57 H57A 0.8505 . O57 H57B 0.8492 . O52 H52A 0.8498 . O52 H52B 0.8503 . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O35 H35 O39 0.82 1.75 2.55(2) 165.4 2 O33 H33 O49 0.82 2.46 2.87(5) 112.0 7_466 O37 H37 O52 0.82 1.84 2.63(4) 162.3 1_455 O39 H39 O58 0.82 1.92 2.63(5) 143.9 2_655 O39 H39 O53 0.82 2.64 3.36(8) 147.0 2_655 O29 H29 O43 0.82 2.26 2.93(4) 139.0 7_566 C12 H12 O19 0.93 2.61 3.46(3) 151.7 7_466 C19 H19 O51 0.93 2.41 3.05(3) 125.7 7_566 C3 H3 O40 0.93 2.66 3.44(3) 141.4 7_566 O55 H55A O5 0.85 2.51 2.96(4) 114.1 1_655 O55 H55A O44 0.85 2.46 3.26(6) 159.2 1_655 C26 H26 O41 0.93 2.60 3.42(4) 146.7 . O58 H58A O35 0.85 3.26 3.43(6) 94.5 1_655 O58 H58A O39 0.85 1.89 2.63(5) 144.5 2_655 O56 H56B O40 0.85 2.82 3.39(4) 126.4 1_655 O56 H56B O53 0.85 2.89 3.15(8) 100.0 2_755 O54 H54A O43 0.85 2.50 3.10(11) 128.3 . O47 H47 O37 0.82 2.65 3.35(5) 145.1 3_445 O53 H53B O58 0.85 1.81 2.61(7) 154.7 . O53 H53B O56 0.85 3.02 3.15(8) 91.2 2_755 O53 H53A O29 0.85 1.89 2.70(7) 159.6 8_565 O57 H57B O27 0.85 2.68 3.21(6) 121.4 5_666 O57 H57B O2 0.85 2.35 3.16(6) 160.6 6_665 O57 H57B O28 0.85 2.86 3.16(6) 103.3 5_666 O52 H52B O4 0.85 2.55 3.00(3) 113.8 7_566 O52 H52B O49 0.85 2.16 2.72(6) 123.0 7_566 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 O11 P1 O17 W6 -50.0(14) . . O24 P1 O17 W6 -177.5(9) 2_556 . O7 P1 O17 W6 66.9(13) . . O11 P1 O17 W7 -179.1(9) . . O24 P1 O17 W7 53.4(13) 2_556 . O7 P1 O17 W7 -62.2(11) . . O17 P1 O7 W2 -176.0(8) . . O11 P1 O7 W2 -56.0(10) . . O24 P1 O7 W2 63.7(10) 2_556 . O17 P1 O7 W3 62.0(11) . . O11 P1 O7 W3 -178.0(9) . . O24 P1 O7 W3 -58.3(11) 2_556 . O17 P1 O7 W1 -57.8(11) . . O11 P1 O7 W1 62.2(11) . . O24 P1 O7 W1 -178.1(8) 2_556 . O20 W6 O15 Na1 -148(2) . . O14 W6 O15 Na1 -55(2) . . O16 W6 O15 Na1 118(2) . . O9 W6 O15 Na1 31(2) . . O15 W6 O14 W5 125.8(19) . . O20 W6 O14 W5 -134.5(18) . . O16 W6 O14 W5 -35(3) . . O9 W6 O14 W5 30.8(18) . . O17 W6 O14 W5 -50.4(18) . . O51 W2 O3 W1 -174.4(10) 2_556 . O8 W2 O3 W1 82.4(10) . . O28 W2 O3 W1 -4(3) 2_556 . O2 W2 O3 W1 -74.6(10) . . O7 W2 O3 W1 -0.9(8) . . O15 W6 O20 W8 100(3) . . O14 W6 O20 W8 -4(3) . . O16 W6 O20 W8 -160(3) . . O9 W6 O20 W8 -76(4) . . O17 W6 O20 W8 -88(3) . . O5 W1 O9 W6 130.5(17) . . O10 W1 O9 W6 29.2(17) . . O4 W1 O9 W6 -127.4(17) . . O3 W1 O9 W6 -44(3) . . O7 W1 O9 W6 -53.9(17) . . O23 W8 O25 W9 -174.0(10) . . O28 W8 O25 W9 86.0(11) . . O22 W8 O25 W9 -2(2) . . O20 W8 O25 W9 -76.5(10) . . O24 W8 O25 W9 3.4(9) . . O5 W1 O10 W5 -124.6(17) . . O9 W1 O10 W5 -24.7(17) . . O4 W1 O10 W5 66(3) . . O3 W1 O10 W5 134.8(17) . . O7 W1 O10 W5 62.1(17) . . O12 W5 O10 W1 126.3(17) . . O14 W5 O10 W1 23.6(17) . . O13 W5 O10 W1 -39(3) . . O19 W5 O10 W1 -133.0(17) . . O11 W5 O10 W1 -60.9(16) . . O26 W9 O21 W7 105(3) . . O18 W9 O21 W7 4(3) 2_556 . O25 W9 O21 W7 -154(3) . . O27 W9 O21 W7 -65(5) . . O24 W9 O21 W7 -81(3) . . O51 W2 O8 W4 129.7(18) 2_556 . O3 W2 O8 W4 -127.6(19) . . O28 W2 O8 W4 30.4(18) 2_556 . O2 W2 O8 W4 -35(3) . . O7 W2 O8 W4 -53.9(18) . . O41 W7 O16 W6 -173.8(10) 5_566 . O6 W7 O16 W6 86.8(10) . . O18 W7 O16 W6 0(2) . . O21 W7 O16 W6 -76.7(10) . . O17 W7 O16 W6 4.7(9) . . O23 W8 O22 W4 -129(2) . 2_556 O25 W8 O22 W4 59(3) . 2_556 O28 W8 O22 W4 -29(2) . 2_556 O20 W8 O22 W4 134(2) . 2_556 O24 W8 O22 W4 54.4(19) . 2_556 O23 W8 O28 W2 133.2(19) . 2_556 O25 W8 O28 W2 -128(2) . 2_556 O22 W8 O28 W2 29(2) . 2_556 O20 W8 O28 W2 -40(4) . 2_556 O24 W8 O28 W2 -55.0(19) . 2_556 O41 W7 O6 W3 124.5(18) 5_566 . O16 W7 O6 W3 -134.9(18) . . O18 W7 O6 W3 22.1(18) . . O21 W7 O6 W3 -49(4) . . O17 W7 O6 W3 -61.6(18) . . C13 N2 C9 C10 0(4) . . Yb1 N2 C9 C10 179.1(17) . . C13 N2 C9 C8 178(2) . . Yb1 N2 C9 C8 -3(3) . . N2 C9 C10 C11 1(4) . . C8 C9 C10 C11 -177(3) . . C9 N2 C13 C12 -1(3) . . Yb1 N2 C13 C12 179.7(16) . . C9 N2 C13 C14 177(2) . . Yb1 N2 C13 C14 -3(3) . . C11 C12 C13 N2 2(3) . . C11 C12 C13 C14 -176(2) . . C2 N1 C6 C5 1(4) . . Yb1 N1 C6 C5 -172.6(18) . . C2 N1 C6 C7 -179(2) . . Yb1 N1 C6 C7 7(3) . . C6 N1 C2 C3 -2(4) . . Yb1 N1 C2 C3 171.9(19) . . C6 N1 C2 C1 -179(2) . . Yb1 N1 C2 C1 -5(3) . . N1 C6 C5 C4 -1(4) . . C7 C6 C5 C4 180(3) . . C9 C10 C11 C12 0(4) . . C13 C12 C11 C10 -1(4) . . C6 C5 C4 C3 2(4) . . Yb1 O30 C1 O29 -174(2) . . Yb1 O30 C1 C2 10(3) . . N1 C2 C1 O29 -179(3) . . C3 C2 C1 O29 4(4) . . N1 C2 C1 O30 -3(4) . . C3 C2 C1 O30 -179(3) . . N1 C2 C1 Yb1 3.4(19) . . C3 C2 C1 Yb1 -173(3) . . C17 C18 C19 C20 1(4) . . O17 P1 O11 W4 -177.3(9) . . O24 P1 O11 W4 -49.3(13) 2_556 . O7 P1 O11 W4 66.3(12) . . O17 P1 O11 W5 52.8(13) . . O24 P1 O11 W5 -179.2(9) 2_556 . O7 P1 O11 W5 -63.6(12) . . Yb1 O40 C21 O39 -175.0(16) . . Yb1 O40 C21 C20 3(3) . . Yb1 O34 C8 O33 -162(2) . . Yb1 O34 C8 C9 6(3) . . N2 C9 C8 O33 167(3) . . C10 C9 C8 O33 -15(4) . . N2 C9 C8 O34 -2(4) . . C10 C9 C8 O34 176(2) . . Na1 O31 C7 O32 110(3) . . Na1 O31 C7 C6 -75(4) . . Na1 O31 C7 Yb1 108(6) . . Yb1 O32 C7 O31 -179(2) . . Yb1 O32 C7 C6 5(3) . . N1 C6 C7 O31 176(3) . . C5 C6 C7 O31 -4(4) . . N1 C6 C7 O32 -8(3) . . C5 C6 C7 O32 172(2) . . N1 C6 C7 Yb1 -4.6(18) . . C5 C6 C7 Yb1 175(2) . . C16 N3 C20 C19 2(4) . . Yb1 N3 C20 C19 179.4(19) . . C16 N3 C20 C21 178(2) . . Yb1 N3 C20 C21 -5(3) . . C18 C19 C20 N3 -3(4) . . C18 C19 C20 C21 -178(3) . . O39 C21 C20 N3 180(2) . . O40 C21 C20 N3 1(3) . . O39 C21 C20 C19 -5(4) . . O40 C21 C20 C19 177(2) . . Yb1 O36 C14 O35 -176.0(17) . . Yb1 O36 C14 C13 -3(3) . . N2 C13 C14 O36 4(3) . . C12 C13 C14 O36 -179(2) . . N2 C13 C14 O35 177(2) . . C12 C13 C14 O35 -5(3) . . Yb1 O38 C15 O37 179(2) . . Yb1 O38 C15 C16 -1(4) . . N1 C2 C3 C4 3(4) . . C1 C2 C3 C4 179(3) . . C5 C4 C3 C2 -2(4) . . C19 C18 C17 C16 1(5) . . C20 N3 C16 C17 0(4) . . Yb1 N3 C16 C17 -177(2) . . C20 N3 C16 C15 177(2) . . Yb1 N3 C16 C15 0(3) . . C18 C17 C16 N3 -1(5) . . C18 C17 C16 C15 -178(3) . . O38 C15 C16 N3 1(4) . . O37 C15 C16 N3 -179(3) . . O38 C15 C16 C17 178(3) . . O37 C15 C16 C17 -2(5) . . C27 C26 C25 C24 2(6) . . C23 C24 C25 C26 -2(5) . . C27 N4 C23 C24 -3(7) . . Na2 N4 C23 C24 -180(3) . . C27 N4 C23 C22 -179(4) . . Na2 N4 C23 C22 4(6) . . C25 C24 C23 N4 2(7) . . C25 C24 C23 C22 178(4) . . O47 C22 C23 N4 -162(6) . . O46 C22 C23 N4 -4(7) . . O47 C22 C23 C24 21(8) . . O46 C22 C23 C24 180(4) . . O47 C22 O46 Na2 159(5) . . C23 C22 O46 Na2 2(7) . . C25 C26 C27 N4 -3(6) . . C25 C26 C27 C28 178(4) . . C23 N4 C27 C26 2(6) . . Na2 N4 C27 C26 -180(3) . . C23 N4 C27 C28 -178(4) . . Na2 N4 C27 C28 -1(5) . . Na1 O44 C28 O45 -173(7) . . Na1 O44 C28 C27 16(13) . . Na2 O45 C28 O44 -175(4) . . Na2 O45 C28 C27 -3(6) . . C26 C27 C28 O44 -6(7) . . N4 C27 C28 O44 175(4) . . C26 C27 C28 O45 -179(4) . . N4 C27 C28 O45 2(6) . .