#------------------------------------------------------------------------------ #$Date: 2021-10-17 01:39:36 +0300 (Sun, 17 Oct 2021) $ #$Revision: 269981 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/37/7243746.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_7243746 loop_ _publ_author_name 'Ying, Jun' 'Jin, Liang' 'Yu, Haiyan' 'Tian, Aixiang' 'Wang, Xiuli' _publ_section_title ; A series of polyoxometalate-based hybrid complexes constructed by a tripodal ligand containing mixed N/O donors ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D1CE01195B _journal_year 2021 _chemical_formula_moiety 'C13 H13 Fe Mo4 N4 O17' _chemical_formula_sum 'C13 H13 Fe Mo4 N4 O17' _chemical_formula_weight 936.88 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _audit_block_doi 10.5517/ccdc.csd.cc26w0gl _audit_creation_date 2020-12-21 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-12-21 deposited with the CCDC. 2021-10-15 downloaded from the CCDC. ; _cell_angle_alpha 83.409(8) _cell_angle_beta 68.107(7) _cell_angle_gamma 73.943(7) _cell_formula_units_Z 2 _cell_length_a 9.589(4) _cell_length_b 11.220(4) _cell_length_c 12.270(5) _cell_measurement_reflns_used 2001 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 28.17 _cell_measurement_theta_min 2.37 _cell_volume 1177.0(8) _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 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 296.15 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.978 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_unetI/netI 0.1070 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.978 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 8507 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.978 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.369 _diffrn_reflns_theta_min 1.789 _exptl_absorpt_coefficient_mu 2.766 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.5134 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0853 before and 0.0616 after correction. The Ratio of minimum to maximum transmission is 0.6885. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.643 _exptl_crystal_description block _exptl_crystal_F_000 898 _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _refine_diff_density_max 3.666 _refine_diff_density_min -2.714 _refine_diff_density_rms 0.376 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 354 _refine_ls_number_reflns 5763 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.007 _refine_ls_R_factor_all 0.1061 _refine_ls_R_factor_gt 0.0734 _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^)+(0.1336P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1890 _refine_ls_wR_factor_ref 0.2142 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4075 _reflns_number_total 5763 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1ce01195b2.cif _cod_data_source_block 2_CCDC1 _cod_database_code 7243746 _shelxl_version_number 2014/6 _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. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All O(H,H) groups 2.a Rotating group: O5(H5A,H5B), O6(H6A,H6B) 2.b Aromatic/amide H refined with riding coordinates: C7(H7), C8(H8), C3(H3), C6(H6), C13(H13), C4(H4), C12(H12), C11(H11), C2(H2) ; _shelx_res_file ; TITL 2_a.res in P-1 REM Old TITL 2 in P-1 REM SHELXT solution in P-1 REM R1 0.107, Rweak 0.003, Alpha 0.053, Orientation as input REM Formula found by SHELXT: C15 N5 O14 Co Mo4 CELL 0.71073 9.589 11.2201 12.2701 83.409 68.107 73.943 ZERR 2 0.0035 0.0042 0.0048 0.008 0.007 0.007 LATT 1 SFAC C H Fe Mo N O UNIT 26 26 2 8 8 34 L.S. 4 0 0 PLAN 20 TEMP 23 FREE Fe1 H5b FREE Fe1 H6a list 4 fmap 2 53 acta OMIT 0 -1 3 OMIT -2 -2 6 OMIT -1 -2 2 OMIT -2 0 1 OMIT 0 1 4 OMIT 2 -2 1 OMIT -3 0 1 OMIT -3 3 2 OMIT -4 3 2 OMIT -1 -2 3 OMIT -2 -1 6 OMIT -2 -3 6 OMIT -2 0 3 OMIT 8 4 14 OMIT -1 0 2 OMIT -1 0 4 OMIT -4 1 5 OMIT -4 0 5 OMIT -2 -3 9 OMIT 2 -2 2 REM REM REM WGHT 0.133600 FVAR 0.29089 MO01 4 0.766663 0.519201 0.678920 11.00000 0.01107 0.01284 = 0.01072 -0.00170 -0.00121 -0.00306 MO02 4 0.507952 0.589413 1.102508 11.00000 0.01272 0.01305 = 0.01192 -0.00057 -0.00280 -0.00341 MO03 4 0.186290 0.662014 1.043774 11.00000 0.01253 0.01597 = 0.01321 -0.00018 -0.00228 -0.00146 MO04 4 0.447490 0.726935 0.799420 11.00000 0.01482 0.01364 = 0.01507 0.00041 -0.00159 -0.00117 FE1 3 0.804848 0.521764 0.373441 11.00000 0.01409 0.01386 = 0.01181 -0.00278 -0.00226 -0.00516 O11 6 0.445167 0.622339 0.967302 11.00000 0.01117 0.01830 = 0.01075 -0.00128 -0.00139 -0.00295 O14 6 0.264247 0.577880 1.164506 11.00000 0.01356 0.02285 = 0.00935 0.00310 -0.00063 -0.00793 O3 6 0.739181 0.565786 0.546939 11.00000 0.01976 0.01984 = 0.01118 -0.00497 0.00070 -0.00354 O15 6 0.481198 0.483887 1.239014 11.00000 0.01492 0.02056 = 0.00947 0.00173 -0.00606 -0.00558 O7 6 0.676769 0.669478 0.756073 11.00000 0.01836 0.01433 = 0.01655 -0.00351 0.00033 -0.00505 O17 6 0.709878 0.543927 1.033656 11.00000 0.01335 0.01617 = 0.02826 -0.00076 -0.00787 -0.00331 O1 6 0.800043 0.337516 0.626400 11.00000 0.03137 0.01187 = 0.02533 0.00109 -0.00998 -0.00594 O10 6 0.241634 0.698061 0.876662 11.00000 0.01979 0.03195 = 0.01647 0.00402 -0.00972 -0.00893 O2 6 0.813854 0.334965 0.439103 11.00000 0.04090 0.01895 = 0.02229 -0.00012 -0.00920 -0.00782 O13 6 0.138748 0.811610 1.090317 11.00000 0.03041 0.01947 = 0.02886 -0.00328 -0.00228 -0.00127 O5 6 0.880185 0.449914 0.207788 11.00000 0.03042 0.02194 = 0.01665 -0.00246 -0.00524 -0.00967 AFIX 7 H5A 2 0.827068 0.398211 0.207426 11.00000 -1.50000 H5B 2 0.831394 0.520757 0.187486 11.00000 -1.50000 AFIX 0 O12 6 0.012567 0.628715 1.070940 11.00000 0.01381 0.03467 = 0.02695 0.00121 -0.00401 -0.01052 O6 6 0.571230 0.553417 0.395918 11.00000 0.02236 0.04543 = 0.02953 -0.00113 -0.01069 -0.01310 AFIX 7 H6A 2 0.594959 0.625936 0.393311 11.00000 -1.50000 H6B 2 0.559440 0.550370 0.328317 11.00000 -1.50000 AFIX 0 O8 6 0.442486 0.761902 0.662061 11.00000 0.02460 0.03262 = 0.02668 0.00560 -0.00211 -0.00905 O4 6 0.960578 0.505733 0.649551 11.00000 0.01428 0.02607 = 0.01748 -0.00180 -0.00069 -0.00710 O16 6 0.476059 0.733199 1.154266 11.00000 0.03082 0.01622 = 0.02729 -0.00786 -0.00403 -0.00539 O9 6 0.427791 0.863987 0.855026 11.00000 0.03374 0.02692 = 0.03865 -0.00519 -0.01373 -0.01182 N3 5 0.765547 -0.109553 0.415543 11.00000 0.02224 0.01427 = 0.02256 -0.00216 -0.00239 -0.00362 N2 5 0.788913 -0.082616 0.800641 11.00000 0.03000 0.01852 = 0.01842 0.00432 -0.00040 -0.01026 N4 5 0.783651 -0.285151 0.339209 11.00000 0.02161 0.02748 = 0.01697 0.00444 -0.00524 -0.00837 N1 5 0.833662 -0.215097 0.930001 11.00000 0.04666 0.03585 = 0.04103 0.01248 -0.02292 -0.00831 C5 1 0.792192 -0.024948 0.687112 11.00000 0.02668 0.01509 = 0.02086 -0.00021 -0.00574 -0.00328 C7 1 0.777828 -0.091334 0.603277 11.00000 0.04118 0.01220 = 0.02943 -0.00644 -0.00611 -0.00736 AFIX 43 H7 2 0.767673 -0.172199 0.619224 11.00000 -1.20000 AFIX 0 C9 1 0.778940 -0.035762 0.497952 11.00000 0.02052 0.01663 = 0.02593 -0.00439 -0.00414 -0.00559 C10 1 0.798001 0.151473 0.558233 11.00000 0.02042 0.01154 = 0.02595 0.00063 -0.00642 -0.00517 C8 1 0.786994 0.086495 0.473937 11.00000 0.02810 0.01617 = 0.01717 0.00211 -0.00167 -0.00393 AFIX 43 H8 2 0.785031 0.123923 0.402674 11.00000 -1.20000 AFIX 0 C3 1 0.859180 -0.195310 0.817916 11.00000 0.03525 0.02718 = 0.02565 0.00492 -0.01414 -0.01146 AFIX 43 H3 2 0.918919 -0.253568 0.759394 11.00000 -1.20000 AFIX 0 C6 1 0.802985 0.096266 0.663857 11.00000 0.02115 0.02340 = 0.01773 -0.00240 -0.00170 -0.00491 AFIX 43 H6 2 0.813518 0.140371 0.718817 11.00000 -1.20000 AFIX 0 C1 1 0.803821 0.286565 0.537165 11.00000 0.02272 0.01664 = 0.01074 -0.00487 0.00536 -0.00468 C13 1 0.836648 -0.230830 0.399177 11.00000 0.02346 0.01827 = 0.02649 -0.00208 -0.00357 -0.00449 AFIX 43 H13 2 0.915165 -0.272002 0.427357 11.00000 -1.20000 AFIX 0 C4 1 0.710267 -0.025416 0.905571 11.00000 0.03934 0.02822 = 0.02571 -0.00279 -0.00767 -0.00681 AFIX 43 H4 2 0.647935 0.055277 0.918362 11.00000 -1.20000 AFIX 0 C12 1 0.676087 -0.190733 0.311710 11.00000 0.04622 0.02469 = 0.03705 -0.00109 -0.02533 -0.00716 AFIX 43 H12 2 0.618600 -0.200047 0.268149 11.00000 -1.20000 AFIX 0 C11 1 0.664656 -0.084136 0.355415 11.00000 0.04197 0.02245 = 0.04120 0.00309 -0.01610 -0.00575 AFIX 43 H11 2 0.600833 -0.007182 0.347029 11.00000 -1.20000 AFIX 0 C2 1 0.739336 -0.106391 0.985874 11.00000 0.04433 0.05267 = 0.02384 0.00129 -0.00821 -0.01308 AFIX 43 H2 2 0.702624 -0.092588 1.066174 11.00000 -1.20000 AFIX 0 HKLF 4 REM 2_a.res in P-1 REM R1 = 0.0734 for 4075 Fo > 4sig(Fo) and 0.1061 for all 5763 data REM 354 parameters refined using 0 restraints END WGHT 0.1336 0.0000 REM Highest difference peak 3.666, deepest hole -2.714, 1-sigma level 0.376 Q1 1 0.9223 0.0442 0.1793 11.00000 0.05 3.67 Q2 1 0.4885 0.7828 0.8235 11.00000 0.05 3.51 Q3 1 0.5553 0.6441 1.1292 11.00000 0.05 3.26 Q4 1 0.1415 0.6019 1.0176 11.00000 0.05 3.19 Q5 1 0.7308 0.4570 0.6580 11.00000 0.05 3.09 Q6 1 0.4665 0.5365 1.0738 11.00000 0.05 3.03 Q7 1 0.7649 0.5406 0.6029 11.00000 0.05 3.02 Q8 1 0.8185 0.5733 0.7103 11.00000 0.05 2.92 Q9 1 0.2368 0.7160 1.0721 11.00000 0.05 2.86 Q10 1 0.1860 0.6449 1.1171 11.00000 0.05 2.62 Q11 1 0.3961 0.6640 0.7699 11.00000 0.05 2.56 Q12 1 0.4474 0.7463 0.7287 11.00000 0.05 2.46 Q13 1 0.7656 0.5009 0.7542 11.00000 0.05 2.39 Q14 1 0.5124 0.6033 1.0226 11.00000 0.05 2.27 Q15 1 0.5025 0.5724 1.1791 11.00000 0.05 2.24 Q16 1 0.2385 0.6657 1.0814 11.00000 0.05 2.15 Q17 1 0.4533 0.7023 0.8786 11.00000 0.05 2.01 Q18 1 0.0748 0.6852 1.0137 11.00000 0.05 1.97 Q19 1 0.7675 0.4679 0.3576 11.00000 0.05 1.95 Q20 1 0.1912 0.6792 0.9598 11.00000 0.05 1.84 ; _shelx_res_checksum 95240 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -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 _atom_site_disorder_assembly _atom_site_disorder_group Mo01 Mo 0.76666(9) 0.51920(7) 0.67892(7) 0.0122(2) Uani 1 1 d . . . . . Mo02 Mo 0.50795(10) 0.58941(7) 1.10251(7) 0.0130(2) Uani 1 1 d . . . . . Mo03 Mo 0.18629(10) 0.66201(8) 1.04377(7) 0.0151(2) Uani 1 1 d . . . . . Mo04 Mo 0.44749(10) 0.72693(8) 0.79942(7) 0.0162(2) Uani 1 1 d . . . . . Fe1 Fe 0.80485(16) 0.52176(13) 0.37344(12) 0.0134(3) Uani 1 1 d . . . . . O11 O 0.4452(8) 0.6223(6) 0.9673(6) 0.0142(14) Uani 1 1 d . . . . . O14 O 0.2642(8) 0.5779(6) 1.1645(6) 0.0159(14) Uani 1 1 d . . . . . O3 O 0.7392(8) 0.5658(6) 0.5469(6) 0.0187(15) Uani 1 1 d . . . . . O15 O 0.4812(8) 0.4839(6) 1.2390(6) 0.0144(14) Uani 1 1 d . . . . . O7 O 0.6768(8) 0.6695(6) 0.7561(6) 0.0179(15) Uani 1 1 d . . . . . O17 O 0.7099(8) 0.5439(6) 1.0337(6) 0.0192(15) Uani 1 1 d . . . . . O1 O 0.8000(9) 0.3375(6) 0.6264(7) 0.0229(16) Uani 1 1 d . . . . . O10 O 0.2416(9) 0.6981(7) 0.8767(6) 0.0216(16) Uani 1 1 d . . . . . O2 O 0.8139(10) 0.3350(7) 0.4391(7) 0.0280(18) Uani 1 1 d . . . . . O13 O 0.1387(10) 0.8116(7) 1.0903(7) 0.0296(19) Uani 1 1 d . . . . . O5 O 0.8802(9) 0.4499(7) 0.2078(6) 0.0231(16) Uani 1 1 d . . . . . H5A H 0.8271 0.3982 0.2074 0.035 Uiso 1 1 d GR . . . . H5B H 0.8314 0.5208 0.1875 0.035 Uiso 1 1 d GR . . . . O12 O 0.0126(8) 0.6287(7) 1.0709(7) 0.0253(17) Uani 1 1 d . . . . . O6 O 0.5712(9) 0.5534(8) 0.3959(7) 0.0310(19) Uani 1 1 d . . . . . H6A H 0.5950 0.6259 0.3933 0.046 Uiso 1 1 d GR . . . . H6B H 0.5594 0.5504 0.3283 0.046 Uiso 1 1 d GR . . . . O8 O 0.4425(9) 0.7619(8) 0.6621(7) 0.0302(19) Uani 1 1 d . . . . . O4 O 0.9606(8) 0.5057(7) 0.6496(6) 0.0202(15) Uani 1 1 d . . . . . O16 O 0.4761(9) 0.7332(7) 1.1543(7) 0.0261(18) Uani 1 1 d . . . . . O9 O 0.4278(10) 0.8640(8) 0.8550(8) 0.0316(19) Uani 1 1 d . . . . . N3 N 0.7655(11) -0.1096(8) 0.4155(8) 0.0214(19) Uani 1 1 d . . . . . N2 N 0.7889(11) -0.0826(8) 0.8006(8) 0.024(2) Uani 1 1 d . . . . . N4 N 0.7837(11) -0.2852(9) 0.3392(8) 0.0225(19) Uani 1 1 d . . . . . N1 N 0.8337(14) -0.2151(10) 0.9300(10) 0.041(3) Uani 1 1 d . . . . . C5 C 0.7922(13) -0.0249(9) 0.6871(9) 0.022(2) Uani 1 1 d . . . . . C7 C 0.7778(15) -0.0913(10) 0.6033(10) 0.029(3) Uani 1 1 d . . . . . H7 H 0.7677 -0.1722 0.6192 0.035 Uiso 1 1 calc R . . . . C9 C 0.7789(13) -0.0358(9) 0.4980(10) 0.022(2) Uani 1 1 d . . . . . C10 C 0.7980(12) 0.1515(9) 0.5582(9) 0.020(2) Uani 1 1 d . . . . . C8 C 0.7870(13) 0.0865(9) 0.4739(9) 0.023(2) Uani 1 1 d . . . . . H8 H 0.7850 0.1239 0.4027 0.028 Uiso 1 1 calc R . . . . C3 C 0.8592(14) -0.1953(11) 0.8179(10) 0.028(3) Uani 1 1 d . . . . . H3 H 0.9189 -0.2536 0.7594 0.034 Uiso 1 1 calc R . . . . C6 C 0.8030(12) 0.0963(10) 0.6639(9) 0.022(2) Uani 1 1 d . . . . . H6 H 0.8135 0.1404 0.7188 0.027 Uiso 1 1 calc R . . . . C1 C 0.8038(12) 0.2866(9) 0.5372(8) 0.020(2) Uani 1 1 d . . . . . C13 C 0.8366(13) -0.2308(10) 0.3992(10) 0.024(2) Uani 1 1 d . . . . . H13 H 0.9152 -0.2720 0.4274 0.029 Uiso 1 1 calc R . . . . C4 C 0.7103(15) -0.0254(12) 0.9056(10) 0.032(3) Uani 1 1 d . . . . . H4 H 0.6479 0.0553 0.9184 0.039 Uiso 1 1 calc R . . . . C12 C 0.6761(16) -0.1907(11) 0.3117(11) 0.033(3) Uani 1 1 d . . . . . H12 H 0.6186 -0.2000 0.2681 0.040 Uiso 1 1 calc R . . . . C11 C 0.6647(16) -0.0841(11) 0.3554(12) 0.036(3) Uani 1 1 d . . . . . H11 H 0.6008 -0.0072 0.3470 0.043 Uiso 1 1 calc R . . . . C2 C 0.7393(17) -0.1064(14) 0.9859(12) 0.041(3) Uani 1 1 d . . . . . H2 H 0.7026 -0.0926 1.0662 0.050 Uiso 1 1 calc R . . . . 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 Mo01 0.0111(4) 0.0128(4) 0.0107(4) -0.0017(3) -0.0012(3) -0.0031(3) Mo02 0.0127(4) 0.0131(4) 0.0119(4) -0.0006(3) -0.0028(3) -0.0034(3) Mo03 0.0125(4) 0.0160(4) 0.0132(4) -0.0002(3) -0.0023(3) -0.0015(3) Mo04 0.0148(4) 0.0136(4) 0.0151(4) 0.0004(3) -0.0016(3) -0.0012(3) Fe1 0.0141(7) 0.0139(7) 0.0118(6) -0.0028(5) -0.0023(5) -0.0052(5) O11 0.011(3) 0.018(3) 0.011(3) -0.001(2) -0.001(3) -0.003(3) O14 0.014(3) 0.023(4) 0.009(3) 0.003(3) -0.001(3) -0.008(3) O3 0.020(4) 0.020(4) 0.011(3) -0.005(3) 0.001(3) -0.004(3) O15 0.015(3) 0.021(3) 0.009(3) 0.002(2) -0.006(3) -0.006(3) O7 0.018(4) 0.014(3) 0.017(3) -0.004(3) 0.000(3) -0.005(3) O17 0.013(4) 0.016(3) 0.028(4) -0.001(3) -0.008(3) -0.003(3) O1 0.031(4) 0.012(3) 0.025(4) 0.001(3) -0.010(3) -0.006(3) O10 0.020(4) 0.032(4) 0.016(4) 0.004(3) -0.010(3) -0.009(3) O2 0.041(5) 0.019(4) 0.022(4) 0.000(3) -0.009(4) -0.008(4) O13 0.030(5) 0.019(4) 0.029(4) -0.003(3) -0.002(4) -0.001(3) O5 0.030(4) 0.022(4) 0.017(4) -0.002(3) -0.005(3) -0.010(3) O12 0.014(4) 0.035(4) 0.027(4) 0.001(3) -0.004(3) -0.011(3) O6 0.022(4) 0.045(5) 0.030(4) -0.001(4) -0.011(4) -0.013(4) O8 0.025(4) 0.033(4) 0.027(4) 0.006(3) -0.002(3) -0.009(4) O4 0.014(4) 0.026(4) 0.017(4) -0.002(3) -0.001(3) -0.007(3) O16 0.031(5) 0.016(4) 0.027(4) -0.008(3) -0.004(3) -0.005(3) O9 0.034(5) 0.027(4) 0.039(5) -0.005(4) -0.014(4) -0.012(4) N3 0.022(5) 0.014(4) 0.023(5) -0.002(3) -0.002(4) -0.004(4) N2 0.030(5) 0.019(4) 0.018(4) 0.004(3) 0.000(4) -0.010(4) N4 0.022(5) 0.027(5) 0.017(4) 0.004(4) -0.005(4) -0.008(4) N1 0.047(7) 0.036(6) 0.041(7) 0.012(5) -0.023(6) -0.008(5) C5 0.027(6) 0.015(5) 0.021(5) 0.000(4) -0.006(4) -0.003(4) C7 0.041(7) 0.012(5) 0.029(6) -0.006(4) -0.006(5) -0.007(5) C9 0.021(6) 0.017(5) 0.026(5) -0.004(4) -0.004(4) -0.006(4) C10 0.020(5) 0.012(4) 0.026(5) 0.001(4) -0.006(4) -0.005(4) C8 0.028(6) 0.016(5) 0.017(5) 0.002(4) -0.002(4) -0.004(4) C3 0.035(7) 0.027(6) 0.026(6) 0.005(4) -0.014(5) -0.011(5) C6 0.021(6) 0.023(5) 0.018(5) -0.002(4) -0.002(4) -0.005(4) C1 0.023(5) 0.017(5) 0.011(4) -0.005(4) 0.005(4) -0.005(4) C13 0.023(6) 0.018(5) 0.026(6) -0.002(4) -0.004(5) -0.004(4) C4 0.039(7) 0.028(6) 0.026(6) -0.003(5) -0.008(5) -0.007(6) C12 0.046(8) 0.025(6) 0.037(7) -0.001(5) -0.025(6) -0.007(6) C11 0.042(8) 0.022(6) 0.041(7) 0.003(5) -0.016(6) -0.006(5) C2 0.044(8) 0.053(8) 0.024(6) 0.001(6) -0.008(6) -0.013(7) 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' 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' 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O14 Mo01 O15 71.5(3) 2_667 2_667 ? O14 Mo01 O1 78.2(3) 2_667 . ? O3 Mo01 O14 155.7(3) . 2_667 ? O3 Mo01 O15 89.4(3) . 2_667 ? O3 Mo01 O7 99.0(3) . . ? O3 Mo01 O1 85.3(3) . . ? O7 Mo01 O14 91.6(3) . 2_667 ? O7 Mo01 O15 77.8(3) . 2_667 ? O7 Mo01 O1 161.6(3) . . ? O1 Mo01 O15 84.4(3) . 2_667 ? O4 Mo01 O14 93.9(3) . 2_667 ? O4 Mo01 O3 105.2(3) . . ? O4 Mo01 O15 165.3(3) . 2_667 ? O4 Mo01 O7 101.0(3) . . ? O4 Mo01 O1 95.1(3) . . ? O11 Mo02 O11 77.4(3) . 2_667 ? O11 Mo02 O14 73.5(3) . . ? O14 Mo02 O11 81.6(2) . 2_667 ? O15 Mo02 O11 139.5(3) . . ? O15 Mo02 O11 74.1(3) . 2_667 ? O15 Mo02 O14 74.3(3) . . ? O17 Mo02 O11 76.8(3) . 2_667 ? O17 Mo02 O11 100.5(3) . . ? O17 Mo02 O14 158.4(3) . . ? O17 Mo02 O15 100.3(3) . . ? O16 Mo02 O11 178.4(3) . 2_667 ? O16 Mo02 O11 104.2(3) . . ? O16 Mo02 O14 98.4(3) . . ? O16 Mo02 O15 104.3(3) . . ? O16 Mo02 O17 103.2(4) . . ? O11 Mo03 O17 70.9(2) . 2_667 ? O14 Mo03 O11 72.8(3) . . ? O14 Mo03 O17 80.4(3) . 2_667 ? O14 Mo03 O10 144.5(3) . . ? O10 Mo03 O11 73.2(3) . . ? O10 Mo03 O17 79.3(3) . 2_667 ? O13 Mo03 O11 100.9(3) . . ? O13 Mo03 O14 98.3(3) . . ? O13 Mo03 O17 171.8(3) . 2_667 ? O13 Mo03 O10 97.7(4) . . ? O12 Mo03 O11 153.5(3) . . ? O12 Mo03 O14 107.0(3) . . ? O12 Mo03 O17 82.8(3) . 2_667 ? O12 Mo03 O10 99.0(3) . . ? O12 Mo03 O13 105.3(4) . . ? O11 Mo04 O15 72.0(2) . 2_667 ? O7 Mo04 O11 83.4(3) . . ? O7 Mo04 O15 72.7(3) . 2_667 ? O10 Mo04 O11 72.8(3) . . ? O10 Mo04 O15 83.0(3) . 2_667 ? O10 Mo04 O7 150.3(3) . . ? O8 Mo04 O11 161.3(3) . . ? O8 Mo04 O15 90.7(3) . 2_667 ? O8 Mo04 O7 98.3(3) . . ? O8 Mo04 O10 98.9(3) . . ? O9 Mo04 O11 93.4(3) . . ? O9 Mo04 O15 162.1(3) . 2_667 ? O9 Mo04 O7 96.0(4) . . ? O9 Mo04 O10 102.8(4) . . ? O9 Mo04 O8 104.9(4) . . ? O3 Fe1 O2 84.6(3) . . ? O3 Fe1 O5 171.2(3) . . ? O3 Fe1 O6 89.1(3) . . ? O3 Fe1 O4 90.6(3) . 2_766 ? O3 Fe1 N4 85.5(3) . 1_565 ? O5 Fe1 O2 86.9(3) . . ? O5 Fe1 O6 93.1(3) . . ? O5 Fe1 O4 87.3(3) . 2_766 ? O5 Fe1 N4 103.0(3) . 1_565 ? O6 Fe1 O2 91.4(3) . . ? O6 Fe1 O4 178.7(3) . 2_766 ? O6 Fe1 N4 88.3(4) . 1_565 ? O4 Fe1 O2 89.9(3) 2_766 . ? O4 Fe1 N4 90.4(3) 2_766 1_565 ? N4 Fe1 O2 170.1(3) 1_565 . ? Mo02 O11 Mo02 102.6(3) . 2_667 ? Mo02 O11 Mo03 104.1(3) . . ? Mo02 O11 Mo04 150.6(4) . . ? Mo03 O11 Mo02 96.6(2) . 2_667 ? Mo03 O11 Mo04 93.8(2) . . ? Mo04 O11 Mo02 98.1(2) . 2_667 ? Mo01 O14 Mo02 104.4(3) 2_667 . ? Mo03 O14 Mo01 150.8(4) . 2_667 ? Mo03 O14 Mo02 104.9(3) . . ? Mo01 O3 Fe1 145.4(4) . . ? Mo01 O15 Mo04 90.7(2) 2_667 2_667 ? Mo02 O15 Mo01 109.2(3) . 2_667 ? Mo02 O15 Mo04 114.7(3) . 2_667 ? Mo01 O7 Mo04 114.6(4) . . ? Mo02 O17 Mo03 115.6(3) . 2_667 ? C1 O1 Mo01 137.0(7) . . ? Mo03 O10 Mo04 114.6(3) . . ? C1 O2 Fe1 132.8(7) . . ? Mo01 O4 Fe1 174.9(4) . 2_766 ? C13 N3 C9 123.4(10) . . ? C13 N3 C11 105.3(9) . . ? C11 N3 C9 130.4(9) . . ? C3 N2 C5 126.1(9) . . ? C3 N2 C4 109.0(10) . . ? C4 N2 C5 124.9(9) . . ? C13 N4 Fe1 115.4(7) . 1_545 ? C13 N4 C12 103.9(9) . . ? C12 N4 Fe1 134.0(8) . 1_545 ? C3 N1 C2 106.6(11) . . ? C7 C5 N2 119.8(10) . . ? C6 C5 N2 120.2(9) . . ? C6 C5 C7 120.0(10) . . ? C9 C7 C5 119.2(10) . . ? C7 C9 N3 116.3(9) . . ? C7 C9 C8 121.5(10) . . ? C8 C9 N3 122.1(10) . . ? C8 C10 C6 121.2(10) . . ? C8 C10 C1 120.6(10) . . ? C6 C10 C1 118.2(9) . . ? C10 C8 C9 118.5(10) . . ? N2 C3 N1 109.8(11) . . ? C5 C6 C10 119.5(10) . . ? O1 C1 C10 113.5(9) . . ? O2 C1 O1 127.0(10) . . ? O2 C1 C10 119.4(9) . . ? N4 C13 N3 112.9(11) . . ? C2 C4 N2 106.6(11) . . ? C11 C12 N4 111.0(11) . . ? C12 C11 N3 106.7(11) . . ? C4 C2 N1 107.9(12) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo01 O14 2.059(7) 2_667 ? Mo01 O3 1.736(7) . ? Mo01 O15 2.217(7) 2_667 ? Mo01 O7 1.854(7) . ? Mo01 O1 2.112(7) . ? Mo01 O4 1.723(7) . ? Mo02 O11 2.484(7) 2_667 ? Mo02 O11 1.932(7) . ? Mo02 O14 2.208(7) . ? Mo02 O15 1.915(7) . ? Mo02 O17 1.748(7) . ? Mo02 O16 1.708(7) . ? Mo03 O11 2.233(7) . ? Mo03 O14 1.939(7) . ? Mo03 O17 2.400(7) 2_667 ? Mo03 O10 1.941(7) . ? Mo03 O13 1.719(8) . ? Mo03 O12 1.711(7) . ? Mo04 O11 2.246(7) . ? Mo04 O15 2.325(7) 2_667 ? Mo04 O7 1.989(7) . ? Mo04 O10 1.946(7) . ? Mo04 O8 1.701(8) . ? Mo04 O9 1.688(8) . ? Fe1 O3 2.060(7) . ? Fe1 O2 2.148(8) . ? Fe1 O5 2.064(7) . ? Fe1 O6 2.084(8) . ? Fe1 O4 2.097(7) 2_766 ? Fe1 N4 2.127(9) 1_565 ? O11 Mo02 2.484(7) 2_667 ? O14 Mo01 2.059(7) 2_667 ? O15 Mo01 2.217(7) 2_667 ? O15 Mo04 2.325(7) 2_667 ? O17 Mo03 2.400(7) 2_667 ? O1 C1 1.277(12) . ? O2 C1 1.243(12) . ? O4 Fe1 2.097(7) 2_766 ? N3 C9 1.440(13) . ? N3 C13 1.343(13) . ? N3 C11 1.376(16) . ? N2 C5 1.460(13) . ? N2 C3 1.293(14) . ? N2 C4 1.355(14) . ? N4 Fe1 2.127(9) 1_545 ? N4 C13 1.313(14) . ? N4 C12 1.369(14) . ? N1 C3 1.308(15) . ? N1 C2 1.377(18) . ? C5 C7 1.404(15) . ? C5 C6 1.382(15) . ? C7 C9 1.367(16) . ? C9 C8 1.387(14) . ? C10 C8 1.382(15) . ? C10 C6 1.382(15) . ? C10 C1 1.521(14) . ? C4 C2 1.317(18) . ? C12 C11 1.327(16) . ?