#------------------------------------------------------------------------------ #$Date: 2018-06-14 15:32:53 +0300 (Thu, 14 Jun 2018) $ #$Revision: 208371 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/66/7046674.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_7046674 loop_ _publ_author_name 'Zhang, Panpan' 'Singh, Vikram' 'Jia, Jiage' 'Zhang, Dongdi' 'Ma, Pengtao' 'Wang, Jingping' 'Niu, Jingyang' _publ_section_title ; Organometallic functionalized non-classical polyoxometalate: synthesis, characterization and electrochemical properties ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/C8DT01712C _journal_year 2018 _chemical_formula_moiety 'C3 Mo12 O48 Re Te2, 13.0[H2O], 8.0[NH4]' _chemical_formula_sum 'C3 H58 Mo12 N8 O61 Re Te2' _chemical_formula_weight 2588.99 _space_group_crystal_system monoclinic _space_group_IT_number 12 _space_group_name_Hall '-C 2y' _space_group_name_H-M_alt 'C 1 2/m 1' _symmetry_space_group_name_Hall '-C 2y' _symmetry_space_group_name_H-M 'C 1 2/m 1' _atom_sites_solution_primary direct _audit_creation_date 2018-05-25 _audit_creation_method ; Olex2 1.2 (compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488) ; _audit_update_record ; 2018-06-09 deposited with the CCDC. 2018-06-13 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 92.232(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 30.620(2) _cell_length_b 20.108(2) _cell_length_c 10.6218(8) _cell_measurement_reflns_used 9975 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 28.29 _cell_measurement_theta_min 2.24 _cell_volume 6535.0(9) _computing_cell_refinement 'SAINT V8.18C (?, 2016)' _computing_data_reduction 'SAINT V8.18C (?, 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 'ShelXS-1997 (Sheldrick, 2008)' _diffrn_ambient_temperature 296.15 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.967 _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 0.0377 _diffrn_reflns_av_unetI/netI 0.0423 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.967 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 20549 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.967 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.295 _diffrn_reflns_theta_min 1.212 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 5.020 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.4132 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1254 before and 0.0394 after correction. The Ratio of minimum to maximum transmission is 0.5541. The \l/2 correction factor is 0.0015.' _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_description block _exptl_crystal_F_000 4340 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.18 _refine_diff_density_max 2.997 _refine_diff_density_min -2.559 _refine_diff_density_rms 0.201 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 319 _refine_ls_number_reflns 8082 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.049 _refine_ls_R_factor_all 0.0410 _refine_ls_R_factor_gt 0.0364 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+38.0401P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0985 _refine_ls_wR_factor_ref 0.1009 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7091 _reflns_number_total 8082 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c8dt01712c2.cif _cod_data_source_block 2 _cod_original_cell_volume 6535.1(10) _cod_database_code 7046674 _shelx_shelxl_version_number 2018/1 _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. ; _shelx_estimated_absorpt_t_max 0.465 _shelx_estimated_absorpt_t_min 0.433 _olex2_refinement_description ; ; _smtbx_masks_special_details ; A solvent mask was calculated and 865.0 electrons were found in a volume of 2843.0\%A^3 in 1 void. This is consistent with the presence of 13[H2O], 8[NH4 ] per formula unit which account for 872.0 electrons. ; _shelx_res_file ; TITL 2 in C2/m 2.res created by SHELXL-2018/1 at 10:38:26 on 25-May-2018 CELL 0.71073 30.6199 20.1085 10.6218 90 92.232 90 ZERR 4 0.0021 0.0021 0.0008 0 0.002 0 LATT 7 SYMM -X,+Y,-Z SFAC C Mo O Re Te UNIT 12 48 192 4 8 L.S. 10 PLAN 10 SIZE 0.2 0.2 0.18 TEMP 23 HTAB fmap 2 acta ABIN OMIT 6 4 4 OMIT -1 1 3 OMIT -4 2 4 OMIT 2 0 0 OMIT 0 0 1 REM REM REM WGHT 0.052700 38.040100 FVAR 0.02086 RE1 4 0.427035 0.000000 0.119952 10.50000 0.02237 0.03050 = 0.04188 0.00000 0.00467 0.00000 TE1 5 0.173481 0.000000 0.172565 10.50000 0.02061 0.01736 = 0.01220 0.00000 0.00088 0.00000 TE2 5 0.280974 0.000000 0.432353 10.50000 0.02142 0.02297 = 0.01534 0.00000 -0.00087 0.00000 MO1 2 0.318754 0.000000 0.082175 10.50000 0.02341 0.02176 = 0.01693 0.00000 0.00237 0.00000 MO2 2 0.193031 0.088353 0.473373 11.00000 0.02343 0.02154 = 0.01491 -0.00397 0.00004 0.00093 MO3 2 0.062540 0.094148 0.165332 11.00000 0.02249 0.02483 = 0.02142 0.00014 -0.00235 0.00268 MO4 2 0.099364 0.000000 0.459848 10.50000 0.02182 0.03044 = 0.01422 0.00000 0.00238 0.00000 MO5 2 0.269956 0.156683 0.205988 11.00000 0.02553 0.01851 = 0.02484 -0.00218 0.00175 -0.00190 MO6 2 0.156048 0.174522 0.148117 11.00000 0.02758 0.01723 = 0.02257 0.00167 -0.00274 0.00080 MO7 2 0.374463 0.084480 0.332680 11.00000 0.02405 0.02767 = 0.03107 -0.00653 -0.00118 -0.00270 O1 3 0.324342 0.000000 0.298835 10.50000 0.01955 0.02357 = 0.01841 0.00000 0.00039 0.00000 O2 3 0.164808 0.000000 0.350954 10.50000 0.02732 0.01754 = 0.01016 0.00000 0.00124 0.00000 O3 3 0.248669 0.071817 0.357640 11.00000 0.02652 0.02112 = 0.02235 -0.00026 0.00459 0.00162 O4 3 0.371526 0.062291 0.132922 11.00000 0.02566 0.02424 = 0.03019 0.00132 0.00191 0.00102 O5 3 0.133885 0.069112 0.138150 11.00000 0.02207 0.01778 = 0.02511 0.00621 -0.00029 -0.00050 O6 3 0.097435 0.172087 0.208437 11.00000 0.02717 0.02451 = 0.02743 -0.00207 -0.00128 0.00440 O7 3 0.222254 0.000000 0.536193 10.50000 0.02457 0.02903 = 0.01743 0.00000 0.00011 0.00000 O8 3 0.172125 0.140356 0.352970 11.00000 0.02761 0.02283 = 0.02211 -0.00053 0.00002 0.00263 O9 3 0.212766 0.133790 0.138935 11.00000 0.02423 0.02461 = 0.02755 -0.00357 0.00015 0.00238 O10 3 0.409092 0.000000 0.317902 10.50000 0.02173 0.03052 = 0.03430 0.00000 0.00041 0.00000 O11 3 0.254550 0.213135 0.317540 11.00000 0.02803 0.02865 = 0.03858 -0.01195 0.00002 -0.00132 O12 3 0.219228 0.140450 0.578319 11.00000 0.03728 0.03423 = 0.02803 -0.01054 -0.00438 -0.00309 O13 3 0.326233 0.138546 0.289288 11.00000 0.02691 0.03018 = 0.03393 -0.00853 0.00086 -0.00080 O14 3 0.143945 0.065356 0.552748 11.00000 0.02434 0.03606 = 0.01840 -0.00740 0.00606 0.00008 O15 3 0.053361 0.000000 0.157024 10.50000 0.02065 0.03142 = 0.02758 0.00000 -0.00282 0.00000 O16 3 0.082153 0.066886 0.363250 11.00000 0.03262 0.03100 = 0.02005 0.00028 -0.00332 0.00022 O17 3 0.056107 0.110036 0.006878 11.00000 0.03645 0.03294 = 0.02842 0.00043 -0.00916 0.00342 O18 3 0.416598 0.138836 0.323105 11.00000 0.03243 0.03751 = 0.05614 -0.01141 0.00030 -0.00504 O19 3 0.327990 0.000000 -0.075357 10.50000 0.03903 0.03542 = 0.01933 0.00000 0.01164 0.00000 O20 3 0.062921 0.000000 0.578263 10.50000 0.03155 0.04782 = 0.02271 0.00000 0.00651 0.00000 O21 3 0.169950 0.252916 0.196423 11.00000 0.04845 0.02081 = 0.04024 -0.00008 -0.00740 -0.00109 O22 3 0.286097 0.206742 0.086589 11.00000 0.04395 0.03122 = 0.03440 0.00470 0.00568 -0.00793 O23 3 0.283709 0.069002 0.101669 11.00000 0.02996 0.02103 = 0.02439 -0.00475 0.00188 0.00006 O24 3 0.145052 0.184271 -0.009726 11.00000 0.03836 0.03161 = 0.02852 0.00933 -0.00726 -0.00424 O25 3 0.365477 0.076364 0.491320 11.00000 0.05194 0.04576 = 0.02772 -0.00418 -0.00305 -0.00093 O26 3 0.014088 0.119711 0.223094 11.00000 0.02738 0.04433 = 0.03896 -0.00535 -0.00105 0.00912 O27 3 0.496894 0.109124 0.142291 11.00000 0.05399 0.07619 = 0.10593 -0.00478 0.01376 -0.01979 O28 3 0.430947 0.000000 -0.166995 10.50000 0.07838 0.11680 = 0.05495 0.00000 0.01387 0.00000 C1 1 0.470324 0.066394 0.133775 11.00000 0.02118 0.03231 = 0.06392 -0.00564 0.00961 -0.00642 C2 1 0.430566 0.000000 -0.051872 10.50000 0.02751 0.04240 = 0.03324 0.00000 0.01786 0.00000 HKLF 4 REM 2 in C2/m REM R1 = 0.0364 for 7091 Fo > 4sig(Fo) and 0.0410 for all 8082 data REM 319 parameters refined using 0 restraints END WGHT 0.0527 38.0551 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 2.997, deepest hole -2.559, 1-sigma level 0.201 Q1 1 0.4543 0.0000 0.0976 10.50000 0.05 3.00 Q2 1 0.4970 0.1501 0.2068 11.00000 0.05 2.85 Q3 1 0.1986 0.0000 0.1588 10.50000 0.05 2.49 Q4 1 0.3424 0.0000 0.0742 10.50000 0.05 2.22 Q5 1 0.3042 0.0000 0.4128 10.50000 0.05 2.02 Q6 1 0.3944 0.0000 0.1401 10.50000 0.05 1.80 Q7 1 0.2184 0.0889 0.4543 11.00000 0.05 1.60 Q8 1 0.2943 0.1563 0.1903 11.00000 0.05 1.41 Q9 1 0.3991 0.0833 0.3133 11.00000 0.05 1.35 Q10 1 0.1655 0.0884 0.4999 11.00000 0.05 1.16 ; 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32 14 2 -2.2397 -0.9203 32 14 3 1.6549 -1.1966 32 14 4 -6.1313 -0.6049 32 16 0 -8.7720 0.4397 32 16 1 1.2779 0.7229 33 1 0 9.9922 -7.3175 33 1 1 -0.5226 -0.6127 33 1 2 -4.4390 3.5994 33 1 3 0.0297 5.3773 33 1 4 -1.9607 3.6119 33 1 5 -6.0114 3.4669 33 1 6 -2.9078 -2.0701 33 1 7 -0.2175 -2.3406 33 3 0 1.5193 0.3752 33 3 1 -2.0444 -0.2134 33 3 2 -2.5555 -0.7016 33 3 3 -3.0020 -3.3139 33 3 4 -7.9171 -2.5463 33 3 5 -0.9138 -2.3121 33 3 6 3.2801 0.6975 33 3 7 -8.9840 -0.7507 33 5 0 -3.4064 0.6557 33 5 1 -0.5223 0.0050 33 5 2 -1.5301 -1.4023 33 5 3 6.5456 -0.8518 33 5 4 3.1544 -0.9135 33 5 5 -1.2182 -0.1777 33 5 6 -9.6727 -1.0962 33 5 7 3.6952 -1.4951 33 7 0 -1.4896 -0.7367 33 7 1 2.4099 0.1120 33 7 2 -0.6474 2.2112 33 7 3 2.8568 -0.0381 33 7 4 -6.1390 0.7727 33 7 5 -8.1133 -0.1217 33 7 6 3.8128 -3.2455 33 9 0 -0.5065 -1.0479 33 9 1 -5.5621 -0.2915 33 9 2 0.4086 -0.8112 33 9 3 0.1126 -0.3894 33 9 4 -0.1237 0.2553 33 9 5 1.1998 0.6532 33 9 6 3.0998 -1.4636 33 11 0 9.2985 1.9716 33 11 1 -3.1221 -0.4928 33 11 2 -0.6604 -3.3253 33 11 3 -2.8915 -2.0214 33 11 4 -0.9962 -0.1757 33 11 5 -15.2366 1.0244 33 13 0 -4.0559 -0.7299 33 13 1 -1.6025 -0.1084 33 13 2 12.6283 1.0513 33 13 3 3.6885 2.6207 33 13 4 -10.2439 0.6867 33 15 0 4.1269 0.2398 33 15 1 -10.6538 1.8717 33 15 2 -1.1516 0.7295 34 0 0 -3.2166 10.2946 34 0 1 11.1872 2.2983 34 0 2 6.4954 6.8338 34 0 3 6.3890 -6.4592 34 0 4 4.3010 -9.5561 34 0 5 -1.3676 -7.7930 34 0 6 2.1826 -1.1981 34 0 7 9.5530 4.4118 34 2 0 -6.1724 0.1491 34 2 1 1.5321 1.0235 34 2 2 10.8805 -4.2668 34 2 3 -4.6875 0.4506 34 2 4 -2.4598 0.8964 34 2 5 -0.7239 1.4805 34 2 6 -7.6477 -0.2565 34 2 7 -5.9337 -1.6067 34 4 0 -1.2475 -2.3862 34 4 1 4.3671 -1.8827 34 4 2 -2.9277 0.5582 34 4 3 4.4043 -0.2068 34 4 4 -1.7891 1.5437 34 4 5 -0.3971 2.3096 34 4 6 -0.7488 1.3637 34 4 7 -1.0285 2.2685 34 6 0 -9.6680 0.4677 34 6 1 0.8239 -1.7612 34 6 2 3.1162 -0.4101 34 6 3 4.1523 -0.5152 34 6 4 8.0915 1.0717 34 6 5 -0.7386 -0.5898 34 6 6 0.0348 1.8451 34 8 0 -0.6501 1.5056 34 8 1 -9.6191 1.3012 34 8 2 3.2895 -0.1374 34 8 3 -0.8512 1.1970 34 8 4 -1.9681 -1.6372 34 8 5 -7.5482 -0.6686 34 8 6 -7.9140 -2.4462 34 10 0 -0.3991 -1.7819 34 10 1 4.4298 -0.3396 34 10 2 2.1097 1.3892 34 10 3 -3.0541 0.4397 34 10 4 -3.9748 -1.0077 34 10 5 -3.6947 -3.3294 34 12 0 2.6315 -0.4364 34 12 1 -2.9782 0.8228 34 12 2 5.7841 0.0559 34 12 3 8.0095 -2.8819 34 12 4 4.4240 -1.4335 34 14 0 -5.2489 0.9699 34 14 1 -1.4854 -1.2772 34 14 2 -12.6936 -1.0378 35 1 0 0.5114 -7.1865 35 1 1 -10.0719 -3.5928 35 1 2 4.3251 -2.1423 35 1 3 8.3321 0.0440 35 1 4 5.8532 2.2802 35 1 5 -4.7322 2.0786 35 1 6 -4.0061 2.9677 35 3 0 -5.7956 3.7260 35 3 1 2.1410 3.3546 35 3 2 -1.3828 1.2601 35 3 3 9.2549 -0.5921 35 3 4 -1.6230 -5.8074 35 3 5 3.4345 -2.5660 35 3 6 7.7339 -0.9268 35 5 0 2.1450 0.1737 35 5 1 -9.4987 1.4024 35 5 2 4.7260 0.8164 35 5 3 1.6952 -1.5944 35 5 4 1.2093 -0.7560 35 5 5 -0.5815 -0.9175 35 5 6 -5.7133 2.1597 35 7 0 4.2812 -0.5717 35 7 1 -1.2179 -0.4798 35 7 2 -11.8156 -0.4328 35 7 3 7.7407 0.2909 35 7 4 4.5550 1.9964 35 7 5 -1.9707 5.2531 35 9 0 7.4335 0.0004 35 9 1 -3.6756 -0.8011 35 9 2 3.7983 -0.4832 35 9 3 9.0882 -0.7657 35 9 4 2.5129 4.8655 35 9 5 -1.6673 -1.1716 35 11 0 -2.1740 1.9751 35 11 1 -2.8415 0.1745 35 11 2 -3.7731 -0.1148 35 11 3 -5.7620 1.5275 35 13 0 -0.7236 -1.5311 35 13 1 -5.6464 -1.7750 36 0 0 -1.7492 4.6519 36 0 1 -3.0640 10.1012 36 0 2 -5.0769 6.9887 36 0 3 0.7716 3.2956 36 0 4 6.5388 -5.5771 36 0 5 12.7376 -8.3848 36 0 6 -1.8353 -4.4683 36 2 0 -6.6759 -1.1991 36 2 1 -4.2714 -2.6798 36 2 2 -0.4574 0.8357 36 2 3 -2.1357 -1.1730 36 2 4 6.2363 3.0074 36 2 5 -3.2360 -1.5417 36 2 6 -5.9453 -4.1403 36 4 0 1.0933 0.0185 36 4 1 -2.8861 -1.7504 36 4 2 -7.6004 -2.2007 36 4 3 5.0330 0.5177 36 4 4 -2.8656 -0.3762 36 4 5 1.1546 -2.3454 36 6 0 -2.5989 -0.4814 36 6 1 -2.2004 -1.2271 36 6 2 -7.6965 0.0645 36 6 3 -1.4231 -0.8400 36 6 4 9.8888 -1.7540 36 6 5 -2.1084 -2.5744 36 8 0 1.1613 0.8771 36 8 1 0.9820 0.9647 36 8 2 -6.9121 1.8563 36 8 3 -6.6045 0.5564 36 8 4 4.6560 -1.9201 36 10 0 -4.7262 0.3527 36 10 1 -2.1752 -0.0961 36 10 2 4.3721 0.2821 36 10 3 1.3450 1.2871 36 12 0 9.0515 2.3285 36 12 1 -0.9149 2.7489 37 1 0 3.5496 -4.8772 37 1 1 -8.4421 -4.5451 37 1 2 -1.7585 -2.6177 37 1 3 -1.3663 -2.1080 37 1 4 0.5888 0.5409 37 1 5 0.8289 3.9478 37 3 0 0.6867 4.8189 37 3 1 -1.7889 5.3152 37 3 2 -6.9542 3.6059 37 3 3 -1.6026 1.9745 37 3 4 1.0230 -0.4252 37 3 5 1.3617 0.2676 37 5 0 0.7584 -0.5126 37 5 1 7.2199 2.4958 37 5 2 -4.1103 0.2441 37 5 3 2.5990 0.6226 37 5 4 -2.8668 0.7538 37 7 0 10.2432 -0.4968 37 7 1 -0.1992 -1.8642 37 7 2 -4.3770 -2.1966 37 7 3 -12.7599 -2.0970 37 7 4 9.3530 -0.5007 37 9 0 -0.1620 1.1566 37 9 1 -0.8830 -1.6851 37 9 2 -6.8628 -3.2655 37 9 3 2.4768 -3.3099 37 11 0 5.9418 -2.1259 38 0 0 5.6545 -0.1858 38 0 1 -5.6983 3.0813 38 0 2 5.5695 7.4226 38 0 3 -7.3032 2.4667 38 2 0 -4.2658 -1.5105 38 2 1 5.2665 -3.5973 38 2 2 -5.8590 -0.4914 38 2 3 1.0726 3.0609 38 2 4 -0.1928 2.5719 38 4 0 -0.6078 1.0643 38 4 1 -1.9369 -0.8668 38 4 2 0.0345 0.6127 38 4 3 -0.5348 0.1191 38 4 4 -0.4929 1.1200 38 6 0 -0.7278 -0.4675 38 6 1 8.2980 0.4460 38 6 2 2.4762 1.2817 38 6 3 -3.5912 0.8829 38 8 1 10.5410 2.3652 38 8 2 4.6248 4.4111 39 1 1 -4.0382 -0.1365 39 1 2 1.7915 -4.5715 39 1 3 2.8320 -4.3758 39 3 1 2.7412 2.2138 39 3 2 -2.4175 1.2241 39 5 2 1.7430 -3.7909 0 0 0 0.0 0.0 ; _shelx_fab_checksum 92068 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' 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 Re1 Re 0.42703(2) 0.000000 0.11995(3) 0.03149(9) Uani 1 2 d S T P Te1 Te 0.17348(2) 0.000000 0.17256(4) 0.01672(10) Uani 1 2 d S T P Te2 Te 0.28097(2) 0.000000 0.43235(4) 0.01995(10) Uani 1 2 d S T P Mo1 Mo 0.31875(2) 0.000000 0.08218(5) 0.02066(13) Uani 1 2 d S T P Mo2 Mo 0.19303(2) 0.08835(2) 0.47337(4) 0.01998(10) Uani 1 1 d . . . Mo3 Mo 0.06254(2) 0.09415(2) 0.16533(4) 0.02300(10) Uani 1 1 d . . . Mo4 Mo 0.09936(2) 0.000000 0.45985(5) 0.02212(13) Uani 1 2 d S T P Mo5 Mo 0.26996(2) 0.15668(2) 0.20599(4) 0.02294(10) Uani 1 1 d . . . Mo6 Mo 0.15605(2) 0.17452(2) 0.14812(4) 0.02256(10) Uani 1 1 d . . . Mo7 Mo 0.37446(2) 0.08448(2) 0.33268(4) 0.02765(11) Uani 1 1 d . . . O1 O 0.32434(16) 0.000000 0.2988(4) 0.0205(10) Uani 1 2 d S T P O2 O 0.16481(16) 0.000000 0.3510(4) 0.0183(9) Uani 1 2 d S T P O3 O 0.24867(12) 0.07182(18) 0.3576(3) 0.0232(7) Uani 1 1 d . . . O4 O 0.37153(12) 0.06229(19) 0.1329(3) 0.0267(8) Uani 1 1 d . . . O5 O 0.13389(11) 0.06911(17) 0.1381(3) 0.0217(7) Uani 1 1 d . . . O6 O 0.09743(12) 0.17209(18) 0.2084(3) 0.0264(8) Uani 1 1 d . . . O7 O 0.22225(17) 0.000000 0.5362(4) 0.0237(10) Uani 1 2 d S T P O8 O 0.17212(12) 0.14036(18) 0.3530(3) 0.0242(7) Uani 1 1 d . . . O9 O 0.21277(12) 0.13379(18) 0.1389(3) 0.0255(8) Uani 1 1 d . . . O10 O 0.40909(18) 0.000000 0.3179(5) 0.0289(11) Uani 1 2 d S T P O11 O 0.25455(13) 0.2131(2) 0.3175(4) 0.0318(9) Uani 1 1 d . . . O12 O 0.21923(14) 0.1405(2) 0.5783(4) 0.0333(9) Uani 1 1 d . . . O13 O 0.32623(13) 0.1385(2) 0.2893(4) 0.0303(8) Uani 1 1 d . . . O14 O 0.14395(12) 0.0654(2) 0.5527(3) 0.0261(8) Uani 1 1 d . . . O15 O 0.05336(17) 0.000000 0.1570(5) 0.0266(11) Uani 1 2 d S T P O16 O 0.08215(13) 0.0669(2) 0.3632(3) 0.0280(8) Uani 1 1 d . . . O17 O 0.05611(13) 0.1100(2) 0.0069(4) 0.0329(9) Uani 1 1 d . . . O18 O 0.41660(15) 0.1388(2) 0.3231(5) 0.0421(10) Uani 1 1 d . . . O19 O 0.32799(19) 0.000000 -0.0754(5) 0.0310(12) Uani 1 2 d S T P O20 O 0.06292(19) 0.000000 0.5783(5) 0.0339(13) Uani 1 2 d S T P O21 O 0.16995(15) 0.2529(2) 0.1964(4) 0.0367(10) Uani 1 1 d . . . O22 O 0.28610(15) 0.2067(2) 0.0866(4) 0.0364(9) Uani 1 1 d . . . O23 O 0.28371(12) 0.06900(18) 0.1017(3) 0.0251(8) Uani 1 1 d . . . O24 O 0.14505(14) 0.1843(2) -0.0097(4) 0.0330(9) Uani 1 1 d . . . O25 O 0.36548(16) 0.0764(2) 0.4913(4) 0.0419(11) Uani 1 1 d . . . O26 O 0.01409(13) 0.1197(2) 0.2231(4) 0.0370(10) Uani 1 1 d . . . O27 O 0.4969(2) 0.1091(3) 0.1423(7) 0.0784(19) Uani 1 1 d . . . O28 O 0.4309(3) 0.000000 -0.1670(8) 0.083(3) Uani 1 2 d S T P C1 C 0.47032(19) 0.0664(3) 0.1338(7) 0.0389(14) Uani 1 1 d . . . C2 C 0.4306(3) 0.000000 -0.0519(8) 0.0339(18) Uani 1 2 d S T P loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.02237(17) 0.03050(18) 0.04188(19) 0.000 0.00467(13) 0.000 Te1 0.0206(2) 0.0174(2) 0.01220(18) 0.000 0.00088(15) 0.000 Te2 0.0214(2) 0.0230(2) 0.01534(19) 0.000 -0.00087(16) 0.000 Mo1 0.0234(3) 0.0218(3) 0.0169(3) 0.000 0.0024(2) 0.000 Mo2 0.0234(2) 0.0215(2) 0.01491(18) -0.00397(14) 0.00004(15) 0.00093(16) Mo3 0.0225(2) 0.0248(2) 0.0214(2) 0.00014(16) -0.00235(16) 0.00268(17) Mo4 0.0218(3) 0.0304(3) 0.0142(2) 0.000 0.0024(2) 0.000 Mo5 0.0255(2) 0.0185(2) 0.0248(2) -0.00218(16) 0.00175(17) -0.00190(17) Mo6 0.0276(2) 0.0172(2) 0.0226(2) 0.00167(15) -0.00274(17) 0.00080(17) Mo7 0.0240(2) 0.0277(2) 0.0311(2) -0.00653(18) -0.00118(18) -0.00270(18) O1 0.020(2) 0.024(3) 0.018(2) 0.000 0.0004(18) 0.000 O2 0.027(3) 0.018(2) 0.0102(19) 0.000 0.0012(17) 0.000 O3 0.0265(19) 0.0211(17) 0.0224(16) -0.0003(14) 0.0046(14) 0.0016(14) O4 0.026(2) 0.0242(19) 0.0302(18) 0.0013(15) 0.0019(15) 0.0010(15) O5 0.0221(18) 0.0178(16) 0.0251(17) 0.0062(13) -0.0003(14) -0.0005(14) O6 0.027(2) 0.0245(19) 0.0274(18) -0.0021(14) -0.0013(15) 0.0044(15) O7 0.025(3) 0.029(3) 0.017(2) 0.000 0.0001(19) 0.000 O8 0.028(2) 0.0228(18) 0.0221(16) -0.0005(14) 0.0000(14) 0.0026(15) O9 0.0242(19) 0.0246(19) 0.0275(18) -0.0036(14) 0.0002(15) 0.0024(15) O10 0.022(3) 0.031(3) 0.034(3) 0.000 0.000(2) 0.000 O11 0.028(2) 0.029(2) 0.039(2) -0.0119(17) 0.0000(16) -0.0013(16) O12 0.037(2) 0.034(2) 0.0280(19) -0.0105(16) -0.0044(16) -0.0031(18) O13 0.027(2) 0.030(2) 0.034(2) -0.0085(16) 0.0009(16) -0.0008(16) O14 0.0243(19) 0.036(2) 0.0184(16) -0.0074(15) 0.0061(14) 0.0001(16) O15 0.021(3) 0.031(3) 0.028(3) 0.000 -0.003(2) 0.000 O16 0.033(2) 0.031(2) 0.0200(16) 0.0003(15) -0.0033(15) 0.0002(17) O17 0.036(2) 0.033(2) 0.0284(19) 0.0004(16) -0.0092(16) 0.0034(18) O18 0.032(2) 0.038(2) 0.056(3) -0.011(2) 0.000(2) -0.0050(19) O19 0.039(3) 0.035(3) 0.019(2) 0.000 0.012(2) 0.000 O20 0.032(3) 0.048(4) 0.023(3) 0.000 0.007(2) 0.000 O21 0.048(3) 0.021(2) 0.040(2) -0.0001(16) -0.0074(19) -0.0011(18) O22 0.044(3) 0.031(2) 0.034(2) 0.0047(17) 0.0057(18) -0.0079(19) O23 0.030(2) 0.0210(18) 0.0244(17) -0.0048(14) 0.0019(15) 0.0001(15) O24 0.038(2) 0.032(2) 0.0285(19) 0.0093(16) -0.0073(17) -0.0042(18) O25 0.052(3) 0.046(3) 0.028(2) -0.0042(19) -0.0031(19) -0.001(2) O26 0.027(2) 0.044(3) 0.039(2) -0.0054(19) -0.0011(17) 0.0091(19) O27 0.054(4) 0.076(4) 0.106(5) -0.005(4) 0.014(3) -0.020(3) O28 0.078(7) 0.117(9) 0.055(5) 0.000 0.014(5) 0.000 C1 0.021(3) 0.032(3) 0.064(4) -0.006(3) 0.010(3) -0.006(2) C2 0.028(4) 0.042(5) 0.033(4) 0.000 0.018(3) 0.000 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' Mo Mo -1.6832 0.6857 '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' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 '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 O4 Re1 O4 72.4(2) 6 . O4 Re1 O10 72.93(15) . . O4 Re1 O10 72.93(15) 6 . C1 Re1 O4 167.8(2) . 6 C1 Re1 O4 167.8(2) 6 . C1 Re1 O4 98.0(2) 6 6 C1 Re1 O4 98.0(2) . . C1 Re1 O10 97.3(2) . . C1 Re1 O10 97.3(2) 6 . C1 Re1 C1 90.3(4) . 6 C2 Re1 O4 98.2(2) . 6 C2 Re1 O4 98.2(2) . . C2 Re1 O10 168.9(3) . . C2 Re1 C1 90.5(3) . . C2 Re1 C1 90.5(3) . 6 O5 Te1 O2 94.54(14) 6 . O5 Te1 O2 94.54(14) . . O5 Te1 O5 95.9(2) 6 . O1 Te2 O7 165.21(19) . . O3 Te2 O1 93.06(14) . . O3 Te2 O1 93.06(14) 6 . O3 Te2 O3 98.5(2) . 6 O3 Te2 O7 77.43(13) . . O3 Te2 O7 77.43(13) 6 . O4 Mo1 O1 73.53(14) . . O4 Mo1 O1 73.53(14) 6 . O4 Mo1 O4 73.3(2) 6 . O19 Mo1 O1 166.2(2) . . O19 Mo1 O4 95.53(19) . 6 O19 Mo1 O4 95.53(19) . . O19 Mo1 O23 103.81(17) . . O19 Mo1 O23 103.81(17) . 6 O23 Mo1 O1 84.54(14) 6 . O23 Mo1 O1 84.54(14) . . O23 Mo1 O4 88.07(16) . . O23 Mo1 O4 88.07(16) 6 6 O23 Mo1 O4 154.38(15) . 6 O23 Mo1 O4 154.38(15) 6 . O23 Mo1 O23 103.1(2) . 6 O3 Mo2 O2 81.38(15) . . O7 Mo2 O2 71.14(14) . . O7 Mo2 O3 73.37(17) . . O8 Mo2 O2 86.06(14) . . O8 Mo2 O3 87.16(15) . . O8 Mo2 O7 151.71(17) . . O8 Mo2 O14 101.87(17) . . O12 Mo2 O2 168.54(17) . . O12 Mo2 O3 96.02(17) . . O12 Mo2 O7 97.41(18) . . O12 Mo2 O8 105.02(19) . . O12 Mo2 O14 103.30(18) . . O14 Mo2 O2 76.72(16) . . O14 Mo2 O3 155.57(16) . . O14 Mo2 O7 89.26(19) . . O6 Mo3 O5 71.68(14) . . O6 Mo3 O16 81.42(15) . . O15 Mo3 O5 85.14(18) . . O15 Mo3 O6 152.51(19) . . O15 Mo3 O16 80.46(18) . . O16 Mo3 O5 80.82(13) . . O17 Mo3 O5 89.48(16) . . O17 Mo3 O6 97.01(18) . . O17 Mo3 O15 97.3(2) . . O17 Mo3 O16 170.18(17) . . O26 Mo3 O5 165.10(17) . . O26 Mo3 O6 98.64(19) . . O26 Mo3 O15 100.7(2) . . O26 Mo3 O16 86.63(18) . . O26 Mo3 O17 103.2(2) . . O14 Mo4 O2 71.47(12) . . O14 Mo4 O2 71.47(12) 6 . O14 Mo4 O14 77.0(2) 6 . O16 Mo4 O2 87.41(15) . . O16 Mo4 O2 87.41(15) 6 . O16 Mo4 O14 157.15(17) . 6 O16 Mo4 O14 88.30(16) . . O16 Mo4 O14 157.14(17) 6 . O16 Mo4 O14 88.29(16) 6 6 O16 Mo4 O16 99.7(2) 6 . O20 Mo4 O2 162.3(2) . . O20 Mo4 O14 94.85(18) . . O20 Mo4 O14 94.85(18) . 6 O20 Mo4 O16 103.84(18) . 6 O20 Mo4 O16 103.84(17) . . O9 Mo5 O3 79.34(14) . . O9 Mo5 O13 154.77(17) . . O9 Mo5 O23 78.75(15) . . O11 Mo5 O3 85.40(16) . . O11 Mo5 O9 98.23(17) . . O11 Mo5 O13 94.15(18) . . O11 Mo5 O23 165.54(17) . . O13 Mo5 O3 79.85(15) . . O13 Mo5 O23 83.79(15) . . O22 Mo5 O3 172.01(17) . . O22 Mo5 O9 98.74(19) . . O22 Mo5 O11 102.6(2) . . O22 Mo5 O13 99.9(2) . . O22 Mo5 O23 91.88(18) . . O23 Mo5 O3 80.15(13) . . O5 Mo6 O8 79.37(13) . . O6 Mo6 O5 72.90(14) . . O6 Mo6 O8 81.20(14) . . O9 Mo6 O5 82.33(14) . . O9 Mo6 O6 149.11(16) . . O9 Mo6 O8 76.25(14) . . O21 Mo6 O5 164.91(17) . . O21 Mo6 O6 98.51(19) . . O21 Mo6 O8 87.14(16) . . O21 Mo6 O9 101.14(19) . . O21 Mo6 O24 103.08(19) . . O24 Mo6 O5 90.83(16) . . O24 Mo6 O6 100.28(18) . . O24 Mo6 O8 169.25(17) . . O24 Mo6 O9 98.21(18) . . O4 Mo7 O1 72.18(15) . . O10 Mo7 O1 73.48(16) . . O10 Mo7 O4 75.62(19) . . O13 Mo7 O1 82.88(15) . . O13 Mo7 O4 82.91(15) . . O13 Mo7 O10 151.89(19) . . O18 Mo7 O1 165.3(2) . . O18 Mo7 O4 94.39(19) . . O18 Mo7 O10 97.8(2) . . O18 Mo7 O13 101.8(2) . . O18 Mo7 O25 105.7(2) . . O25 Mo7 O1 87.26(19) . . O25 Mo7 O4 159.18(19) . . O25 Mo7 O10 95.8(2) . . O25 Mo7 O13 98.1(2) . . Te2 O1 Mo1 133.7(2) . . Te2 O1 Mo7 110.41(15) . . Te2 O1 Mo7 110.41(15) . 6 Mo1 O1 Mo7 100.30(15) . . Mo1 O1 Mo7 100.30(15) . 6 Mo7 O1 Mo7 94.78(18) 6 . Te1 O2 Mo2 118.94(14) . 6 Te1 O2 Mo2 118.94(14) . . Te1 O2 Mo4 129.6(2) . . Mo2 O2 Mo2 98.42(16) . 6 Mo2 O2 Mo4 91.72(13) 6 . Mo2 O2 Mo4 91.71(13) . . Te2 O3 Mo2 106.68(16) . . Te2 O3 Mo5 130.83(17) . . Mo2 O3 Mo5 120.08(15) . . Re1 O4 Mo7 100.52(15) . . Mo1 O4 Re1 104.00(16) . . Mo1 O4 Mo7 112.13(17) . . Te1 O5 Mo3 139.38(18) . . Te1 O5 Mo6 120.25(17) . . Mo6 O5 Mo3 94.35(13) . . Mo6 O6 Mo3 116.91(18) . . Mo2 O7 Te2 101.13(15) 6 . Mo2 O7 Te2 101.13(15) . . Mo2 O7 Mo2 116.7(2) 6 . Mo2 O8 Mo6 156.9(2) . . Mo5 O9 Mo6 133.6(2) . . Mo7 O10 Re1 103.13(18) 6 . Mo7 O10 Re1 103.13(18) . . Mo7 O10 Mo7 115.2(3) . 6 Mo7 O13 Mo5 153.8(2) . . Mo2 O14 Mo4 118.31(17) . . Mo3 O15 Mo3 162.5(3) 6 . Mo4 O16 Mo3 143.2(2) . . Mo1 O23 Mo5 147.2(2) . . O27 C1 Re1 178.6(6) . . O28 C2 Re1 177.2(8) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Re1 O4 2.120(4) 6 Re1 O4 2.120(4) . Re1 O10 2.194(6) . Re1 C1 1.883(6) 6 Re1 C1 1.883(6) . Re1 C2 1.832(8) . Te1 O2 1.924(4) . Te1 O5 1.871(3) 6 Te1 O5 1.871(3) . Te2 O1 1.980(5) . Te2 O3 1.906(4) . Te2 O3 1.906(4) 6 Te2 O7 2.146(5) . Mo1 O1 2.301(5) . Mo1 O4 2.098(4) 6 Mo1 O4 2.098(4) . Mo1 O19 1.708(5) . Mo1 O23 1.771(4) 6 Mo1 O23 1.771(4) . Mo2 O2 2.347(3) . Mo2 O3 2.165(3) . Mo2 O7 2.087(3) . Mo2 O8 1.754(4) . Mo2 O12 1.707(4) . Mo2 O14 1.812(4) . Mo3 O5 2.271(4) . Mo3 O6 1.941(4) . Mo3 O15 1.9155(9) . Mo3 O16 2.232(3) . Mo3 O17 1.717(4) . Mo3 O26 1.707(4) . Mo4 O2 2.352(5) . Mo4 O14 2.112(4) 6 Mo4 O14 2.112(4) . Mo4 O16 1.760(4) 6 Mo4 O16 1.760(4) . Mo4 O20 1.714(5) . Mo5 O3 2.452(3) . Mo5 O9 1.921(4) . Mo5 O11 1.720(4) . Mo5 O13 1.941(4) . Mo5 O22 1.707(4) . Mo5 O23 2.133(4) . Mo6 O5 2.227(3) . Mo6 O6 1.930(4) . Mo6 O8 2.316(3) . Mo6 O9 1.926(4) . Mo6 O21 1.707(4) . Mo6 O24 1.708(4) . Mo7 O1 2.308(3) . Mo7 O4 2.167(4) . Mo7 O10 2.012(3) . Mo7 O13 1.877(4) . Mo7 O18 1.697(4) . Mo7 O25 1.726(4) . O27 C1 1.184(8) . O28 C2 1.223(11) . loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.705 -0.761 -0.869 2840.5 845.0 '6.5 H2O, 4 NH4 '