#------------------------------------------------------------------------------ #$Date: 2021-10-17 01:39:36 +0300 (Sun, 17 Oct 2021) $ #$Revision: 269981 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/37/7243748.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_7243748 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 H12 Mo4 N4 O17 Zn' _chemical_formula_sum 'C13 H12 Mo4 N4 O17 Zn' _chemical_formula_weight 945.40 _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 _atom_sites_solution_primary dual _audit_block_doi 10.5517/ccdc.csd.cc26rrnd _audit_creation_date 2020-12-07 _audit_creation_method ; Olex2 1.3-alpha (compiled 2019.10.31 svn.r3677 for OlexSys, GUI svn.r5972) ; _audit_update_record ; 2020-12-07 deposited with the CCDC. 2021-10-15 downloaded from the CCDC. ; _cell_angle_alpha 83.4150(10) _cell_angle_beta 68.1790(10) _cell_angle_gamma 73.8600(10) _cell_formula_units_Z 2 _cell_length_a 9.6183(3) _cell_length_b 11.1742(4) _cell_length_c 12.2597(4) _cell_measurement_reflns_used 4091 _cell_measurement_temperature 296.15 _cell_measurement_theta_max 28.39 _cell_measurement_theta_min 2.36 _cell_volume 1174.92(7) _computing_cell_refinement 'SAINT V8.18C (?, 2016)' _computing_data_reduction 'SAINT V8.18C (?, 2016)' _computing_molecular_graphics 'Olex2 1.3-alpha (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3-alpha (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 296.15 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.993 _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 0.0183 _diffrn_reflns_av_unetI/netI 0.0364 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 8765 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.397 _diffrn_reflns_theta_min 1.789 _diffrn_source_current 30.0 _diffrn_source_power 1.2 _diffrn_source_voltage 40.0 _exptl_absorpt_coefficient_mu 3.174 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.5884 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0733 before and 0.0270 after correction. The Ratio of minimum to maximum transmission is 0.7891. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.672 _exptl_crystal_description block _exptl_crystal_F_000 904 _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.633 _refine_diff_density_min -0.660 _refine_diff_density_rms 0.126 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 354 _refine_ls_number_reflns 5854 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 10.747 _refine_ls_R_factor_all 0.0334 _refine_ls_R_factor_gt 0.0257 _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^)+(0.0197P)^2^+1.4576P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.0587 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5050 _reflns_number_total 5854 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1ce01195b2.cif _cod_data_source_block 2_CCDC3 _cod_database_code 7243748 _shelx_shelxl_version_number 2018/3 _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) groups, All O(H,H) groups 2. Restrained distances O17-O4 3.5 with sigma of 0.01 3.a Rotating group: O15(H15), O14(H14A,H14B) 3.b Aromatic/amide H refined with riding coordinates: C6(H6), C12(H12), C9(H9), C5(H5), C1(H1), C11(H11), C13(H13), C2(H2), C3(H3) ; _shelx_res_file ; TITL 2_a.res in P-1 2.res created by SHELXL-2018/3 at 10:51:19 on 07-Dec-2020 REM Old TITL 2_a.res in P-1 REM SHELXT solution in P-1 REM R1 0.065, Rweak 0.005, Alpha 0.039, Orientation as input REM Formula found by SHELXT: C6AA Mo5 N8 O12 CELL 0.71073 9.6183 11.1742 12.2597 83.415 68.179 73.86 ZERR 2 0.0003 0.0004 0.0004 0.001 0.001 0.001 LATT 1 SFAC C H Mo N O Zn UNIT 26 24 8 8 34 2 DFIX 3.5 0.01 O17 O4 L.S. 15 0 0 PLAN 80 TEMP 23 CONF list 4 ABIN MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.019700 1.457600 FVAR 0.33354 MO01 3 0.233896 0.980225 0.321420 11.00000 0.01296 0.01071 = 0.00881 0.00059 -0.00400 -0.00504 MO02 3 0.492719 0.909865 -0.102660 11.00000 0.01361 0.01078 = 0.00972 0.00131 -0.00582 -0.00518 MO03 3 0.553283 0.773183 0.200490 11.00000 0.01539 0.01112 = 0.01312 0.00274 -0.00529 -0.00337 MO04 3 0.812969 0.838757 -0.043734 11.00000 0.01257 0.01352 = 0.01128 0.00193 -0.00569 -0.00316 ZN1 6 0.198404 0.976384 0.629432 11.00000 0.02114 0.01607 = 0.01696 -0.00205 -0.00881 -0.00671 O6 5 0.554749 0.878291 0.032115 11.00000 0.01422 0.01521 = 0.01059 0.00274 -0.00554 -0.00514 O4 5 0.734128 0.921332 -0.163429 11.00000 0.01509 0.01673 = 0.01089 0.00380 -0.00622 -0.00538 O13 5 0.262006 0.934033 0.452730 11.00000 0.02379 0.01606 = 0.01190 0.00018 -0.00621 -0.00631 O1 5 0.519281 1.014966 -0.239491 11.00000 0.01632 0.01635 = 0.01027 0.00252 -0.00781 -0.00629 O8 5 0.757399 0.802752 0.123864 11.00000 0.01690 0.01929 = 0.01497 0.00452 -0.00893 -0.00601 O11 5 0.325432 0.830879 0.242582 11.00000 0.01373 0.01411 = 0.01494 -0.00033 -0.00544 -0.00568 O3 5 0.292043 0.955398 -0.033441 11.00000 0.01641 0.01772 = 0.01723 -0.00019 -0.00620 -0.00654 O12 5 0.040763 0.992067 0.352097 11.00000 0.01593 0.02082 = 0.02139 -0.00222 -0.00638 -0.00702 O16 5 0.184258 0.165160 0.561034 11.00000 0.05043 0.01456 = 0.01626 0.00251 -0.01408 -0.01449 O7 5 0.986204 0.874007 -0.071641 11.00000 0.01731 0.02566 = 0.02399 0.00474 -0.00722 -0.00794 O15 5 0.120029 1.051028 0.792473 11.00000 0.03380 0.02189 = 0.01679 0.00443 -0.01160 -0.01390 AFIX 7 H15 2 0.096572 0.995208 0.846123 11.00000 -1.50000 AFIX 0 O5 5 0.862679 0.691094 -0.090668 11.00000 0.03141 0.01650 = 0.02752 -0.00241 -0.01068 -0.00284 O10 5 0.558217 0.739010 0.337901 11.00000 0.02790 0.02856 = 0.02032 0.00623 -0.01158 -0.00545 O14 5 0.431621 0.944850 0.605056 11.00000 0.03398 0.05105 = 0.02387 -0.00431 -0.01708 -0.01981 AFIX 7 H14A 2 0.472621 0.969367 0.645868 11.00000 -1.50000 H14B 2 0.451591 0.908234 0.554704 11.00000 -1.50000 AFIX 0 O9 5 0.574592 0.634413 0.145305 11.00000 0.03037 0.01501 = 0.03038 -0.00349 -0.00668 -0.00534 O2 5 0.525777 0.765868 -0.153402 11.00000 0.02431 0.01632 = 0.02259 -0.00178 -0.00771 -0.00675 N3 4 0.212222 0.582020 0.201613 11.00000 0.02826 0.01592 = 0.01728 0.00544 -0.01162 -0.00862 N2 4 0.232785 0.610128 0.585334 11.00000 0.02852 0.01204 = 0.02078 -0.00054 -0.01195 -0.00658 N1 4 0.215904 0.785341 0.662045 11.00000 0.02599 0.01892 = 0.02121 -0.00224 -0.00944 -0.00946 C8 1 0.194699 0.213542 0.463367 11.00000 0.01794 0.01625 = 0.01439 -0.00043 -0.00676 -0.00836 C10 1 0.209680 0.524894 0.312727 11.00000 0.02104 0.01457 = 0.01697 0.00220 -0.00880 -0.00415 C6 1 0.223683 0.592299 0.394798 11.00000 0.02694 0.01054 = 0.02281 0.00218 -0.01033 -0.00799 AFIX 43 H6 2 0.234973 0.673106 0.377912 11.00000 -1.20000 AFIX 0 N4 4 0.167120 0.717205 0.070365 11.00000 0.04802 0.03318 = 0.03489 0.01305 -0.02420 -0.01501 C7 1 0.201293 0.347791 0.442439 11.00000 0.01830 0.00994 = 0.01662 -0.00105 -0.00607 -0.00395 C12 1 0.137836 0.698821 0.184494 11.00000 0.03291 0.01809 = 0.03237 0.00598 -0.01831 -0.00604 AFIX 43 H12 2 0.076081 0.757161 0.242814 11.00000 -1.20000 AFIX 0 C9 1 0.197758 0.403529 0.335658 11.00000 0.02185 0.01353 = 0.01825 -0.00065 -0.00834 -0.00760 AFIX 43 H9 2 0.187478 0.359503 0.280353 11.00000 -1.20000 AFIX 0 C5 1 0.210551 0.414074 0.528162 11.00000 0.02257 0.01502 = 0.01570 0.00168 -0.00802 -0.00562 AFIX 43 H5 2 0.210098 0.377394 0.600288 11.00000 -1.20000 AFIX 0 C1 1 0.163626 0.733001 0.599510 11.00000 0.02175 0.01472 = 0.02967 -0.00239 -0.01251 -0.00523 AFIX 43 H1 2 0.088147 0.775635 0.568844 11.00000 -1.20000 AFIX 0 C4 1 0.220466 0.536446 0.502660 11.00000 0.02031 0.01188 = 0.02119 -0.00153 -0.00966 -0.00458 C11 1 0.290417 0.523913 0.094034 11.00000 0.03976 0.02547 = 0.01950 0.00026 -0.00812 -0.00798 AFIX 43 H11 2 0.350953 0.442351 0.080590 11.00000 -1.20000 AFIX 0 C13 1 0.261636 0.608646 0.012684 11.00000 0.05277 0.04602 = 0.01732 0.00648 -0.00974 -0.01909 AFIX 43 H13 2 0.298775 0.596261 -0.067928 11.00000 -1.20000 AFIX 0 C2 1 0.324189 0.690320 0.689786 11.00000 0.04269 0.02364 = 0.02778 0.00372 -0.02417 -0.01311 AFIX 43 H2 2 0.381418 0.699336 0.733609 11.00000 -1.20000 AFIX 0 C3 1 0.335441 0.581784 0.644097 11.00000 0.04349 0.01779 = 0.03484 0.00643 -0.02715 -0.00683 AFIX 43 H3 2 0.399389 0.504038 0.650991 11.00000 -1.20000 AFIX 0 O17 5 0.199459 0.163236 0.373017 11.00000 0.03276 0.01092 = 0.01421 -0.00076 -0.01072 -0.00817 HKLF 4 REM 2_a.res in P-1 REM wR2 = 0.0587, GooF = S = 1.049, Restrained GooF = 10.747 for all data REM R1 = 0.0257 for 5050 Fo > 4sig(Fo) and 0.0334 for all 5854 data REM 354 parameters refined using 1 restraints END WGHT 0.0196 1.4638 REM Highest difference peak 0.633, deepest hole -0.660, 1-sigma level 0.126 Q1 1 0.1153 0.7734 0.0264 11.00000 0.05 0.63 Q2 1 0.1876 0.5590 0.4647 11.00000 0.05 0.56 Q3 1 0.0841 1.0177 0.3879 11.00000 0.05 0.54 Q4 1 0.1456 0.9464 0.3610 11.00000 0.05 0.54 Q5 1 0.1557 1.1010 0.8210 11.00000 0.05 0.53 Q6 1 0.5175 0.6603 0.2020 11.00000 0.05 0.52 Q7 1 0.7870 0.6936 0.1605 11.00000 0.05 0.51 Q8 1 0.4860 0.9945 0.5411 11.00000 0.05 0.50 Q9 1 0.0379 0.7986 0.1944 11.00000 0.05 0.49 Q10 1 0.6410 0.8793 0.0361 11.00000 0.05 0.49 Q11 1 0.6246 0.6820 0.1186 11.00000 0.05 0.48 Q12 1 0.4627 0.8051 -0.1163 11.00000 0.05 0.48 Q13 1 0.1560 0.8052 0.0373 11.00000 0.05 0.48 Q14 1 0.0986 0.9417 0.3767 11.00000 0.05 0.47 Q15 1 0.1929 0.8762 0.2980 11.00000 0.05 0.47 Q16 1 0.1836 1.1157 0.7869 11.00000 0.05 0.46 Q17 1 0.5765 0.8064 -0.1825 11.00000 0.05 0.46 Q18 1 0.7600 0.9436 -0.1927 11.00000 0.05 0.46 Q19 1 0.8759 0.7406 -0.0667 11.00000 0.05 0.46 Q20 1 0.2396 0.9904 0.4246 11.00000 0.05 0.45 Q21 1 0.1559 0.4756 0.5214 11.00000 0.05 0.45 Q22 1 0.1990 0.1361 0.4014 11.00000 0.05 0.44 Q23 1 0.9429 0.6207 0.0617 11.00000 0.05 0.44 Q24 1 0.1761 0.4462 0.7568 11.00000 0.05 0.43 Q25 1 0.6369 0.8186 0.1615 11.00000 0.05 0.43 Q26 1 0.7548 0.8012 -0.0210 11.00000 0.05 0.43 Q27 1 0.1555 0.7187 0.1070 11.00000 0.05 0.43 Q28 1 0.7816 0.7218 -0.0710 11.00000 0.05 0.43 Q29 1 0.2142 0.5401 0.1000 11.00000 0.05 0.42 Q30 1 0.4991 0.8804 0.0560 11.00000 0.05 0.42 Q31 1 0.1745 0.3917 0.4862 11.00000 0.05 0.42 Q32 1 0.2072 0.6465 0.2023 11.00000 0.05 0.41 Q33 1 0.1466 0.4810 0.3368 11.00000 0.05 0.41 Q34 1 0.3957 0.8051 0.2591 11.00000 0.05 0.41 Q35 1 0.3618 0.9596 -0.0446 11.00000 0.05 0.41 Q36 1 0.1907 0.5729 0.6125 11.00000 0.05 0.41 Q37 1 0.5375 0.9789 -0.1941 11.00000 0.05 0.40 Q38 1 1.0182 0.8145 -0.0834 11.00000 0.05 0.40 Q39 1 0.2471 0.5053 -0.1727 11.00000 0.05 0.40 Q40 1 0.2538 0.6532 0.0318 11.00000 0.05 0.40 Q41 1 0.3395 0.9786 0.4118 11.00000 0.05 0.40 Q42 1 0.4563 1.0012 0.0606 11.00000 0.05 0.40 Q43 1 0.9118 0.8707 -0.0777 11.00000 0.05 0.40 Q44 1 0.1425 0.9247 0.6627 11.00000 0.05 0.40 Q45 1 0.9730 0.6824 -0.1390 11.00000 0.05 0.39 Q46 1 0.7197 0.7282 0.1336 11.00000 0.05 0.39 Q47 1 0.3433 0.2064 0.3206 11.00000 0.05 0.39 Q48 1 0.1828 0.6897 0.0033 11.00000 0.05 0.38 Q49 1 0.1004 1.0168 0.3490 11.00000 0.05 0.38 Q50 1 0.5369 0.7597 0.3989 11.00000 0.05 0.38 Q51 1 0.2627 1.0474 -0.0580 11.00000 0.05 0.38 Q52 1 0.6132 0.5841 0.1530 11.00000 0.05 0.38 Q53 1 0.1651 0.3800 0.4006 11.00000 0.05 0.38 Q54 1 0.5829 0.9813 -0.2777 11.00000 0.05 0.38 Q55 1 0.2429 0.8980 0.4685 11.00000 0.05 0.38 Q56 1 0.6050 0.7385 -0.0347 11.00000 0.05 0.38 Q57 1 0.7766 0.5464 0.1137 11.00000 0.05 0.37 Q58 1 0.8220 0.6424 -0.1610 11.00000 0.05 0.37 Q59 1 0.4641 0.9187 0.0450 11.00000 0.05 0.37 Q60 1 0.3058 0.8268 0.8157 11.00000 0.05 0.37 Q61 1 0.0632 1.1066 0.7760 11.00000 0.05 0.37 Q62 1 0.1763 0.8330 0.6957 11.00000 0.05 0.37 Q63 1 0.2993 0.6008 -0.0196 11.00000 0.05 0.37 Q64 1 0.1656 0.8799 0.5639 11.00000 0.05 0.37 Q65 1 0.2507 0.9597 -0.0261 11.00000 0.05 0.37 Q66 1 0.5450 0.9165 -0.0183 11.00000 0.05 0.37 Q67 1 0.5720 0.9344 0.4790 11.00000 0.05 0.37 Q68 1 0.6047 0.6579 0.1965 11.00000 0.05 0.37 Q69 1 0.9843 0.8820 -0.1178 11.00000 0.05 0.36 Q70 1 0.0963 1.0783 0.7597 11.00000 0.05 0.36 Q71 1 0.2992 0.8616 0.3030 11.00000 0.05 0.36 Q72 1 0.3955 0.9284 0.6039 11.00000 0.05 0.36 Q73 1 0.0361 0.4877 0.2229 11.00000 0.05 0.36 Q74 1 0.1317 0.7975 0.5152 11.00000 0.05 0.36 Q75 1 0.3847 0.7583 0.2231 11.00000 0.05 0.36 Q76 1 0.3023 0.6359 0.3384 11.00000 0.05 0.36 Q77 1 0.3825 1.0385 0.6136 11.00000 0.05 0.36 Q78 1 0.1603 0.3960 0.3160 11.00000 0.05 0.36 Q79 1 0.0608 0.2743 0.5777 11.00000 0.05 0.36 Q80 1 0.2236 0.1012 0.3620 11.00000 0.05 0.35 ; _shelx_res_checksum 9096 _shelx_fab_file ; -11 -8 1 -0.0165 -0.0651 -11 -7 1 -0.0590 0.0651 -11 -6 1 0.2180 -0.0624 -11 -6 2 -0.0101 -0.0991 -11 -5 1 -0.3746 0.0490 -11 -5 2 0.0981 0.0687 -11 -4 1 0.4088 -0.0253 -11 -4 2 -0.2652 -0.0291 -11 -3 1 -0.2528 0.0035 -11 -3 2 0.4583 0.0000 -11 -2 1 -0.0418 0.0007 -11 -2 2 -0.5849 0.0101 -11 -1 1 0.3184 0.0182 -11 -1 2 0.5671 -0.0109 -11 0 1 -0.4163 -0.0486 -11 1 1 0.2869 0.0678 -10 -10 1 -0.0324 -0.0886 -10 -9 1 0.1142 0.0626 -10 -9 2 -0.0489 0.0666 -10 -8 1 -0.1596 -0.0382 -10 -8 2 0.1850 -0.0712 -10 -8 3 0.2148 -0.0553 -10 -7 1 0.1054 0.0229 -10 -7 2 -0.3468 0.0788 -10 -7 3 -0.2402 0.0838 -10 -6 1 0.0860 -0.0163 -10 -6 2 0.4810 -0.0759 -10 -6 3 0.1923 -0.0858 -10 -6 4 -0.0913 -0.0278 -10 -5 1 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-0.0783 -0.0273 10 2 4 0.2348 -0.0275 10 2 5 0.1567 0.0115 10 2 6 0.3230 0.0305 10 2 7 0.3751 0.0114 10 2 8 -0.1706 -0.0102 10 2 9 -0.7148 -0.0204 10 2 10 -0.6495 -0.0198 10 2 11 -0.3599 0.0125 10 2 12 -0.2678 0.0610 10 3 0 -0.0837 -0.0101 10 3 1 1.0632 -0.0144 10 3 2 0.9437 0.0074 10 3 3 -0.0713 0.0242 10 3 4 -0.4935 0.0086 10 3 5 -0.4242 -0.0158 10 3 6 -0.4729 -0.0095 10 3 7 -0.2011 0.0109 10 3 8 0.5065 0.0068 10 3 9 0.7464 -0.0010 10 3 10 0.2924 0.0083 10 3 11 0.0085 -0.0136 10 3 12 0.1500 -0.0746 10 3 13 0.0473 -0.0851 10 4 0 -0.3722 -0.0051 10 4 1 -1.3236 -0.0093 10 4 2 -0.6986 -0.0092 10 4 3 0.4270 -0.0034 10 4 4 0.6057 0.0042 10 4 5 0.3920 0.0046 10 4 6 0.3930 -0.0099 10 4 7 0.0581 -0.0167 10 4 8 -0.5229 0.0063 10 4 9 -0.4586 0.0196 10 4 10 0.0824 -0.0024 10 4 11 0.1613 0.0061 10 4 12 -0.1004 0.0682 10 4 13 0.1106 0.0850 10 4 14 0.6361 0.0138 10 5 0 0.7081 0.0244 10 5 1 1.1444 0.0265 10 5 2 0.1369 0.0006 10 5 3 -0.6927 -0.0131 10 5 4 -0.4102 -0.0012 10 5 5 -0.1121 0.0120 10 5 6 -0.2441 0.0192 10 5 7 -0.0670 0.0136 10 5 8 0.2759 -0.0171 10 5 9 0.0782 -0.0308 10 5 10 -0.2821 0.0029 10 5 11 -0.1378 0.0109 10 5 12 0.0743 -0.0460 10 5 13 -0.2564 -0.0709 10 5 14 -0.6713 -0.0074 10 6 0 -0.7596 -0.0371 10 6 1 -0.6219 -0.0361 10 6 2 0.4304 0.0024 10 6 3 0.6776 0.0131 10 6 4 -0.0183 -0.0088 10 6 5 -0.2371 -0.0199 10 6 6 0.1228 -0.0210 10 6 7 0.1660 -0.0138 10 6 8 0.0244 0.0216 10 6 9 0.1773 0.0379 10 6 10 0.2585 -0.0076 10 6 11 0.0062 -0.0327 10 6 12 -0.0607 0.0189 10 6 13 0.2837 0.0513 10 7 0 0.5463 0.0374 10 7 1 0.0233 0.0443 10 7 2 -0.7534 0.0102 10 7 3 -0.4110 -0.0015 10 7 4 0.4757 0.0095 10 7 5 0.5306 0.0138 10 7 6 0.0111 0.0250 10 7 7 -0.1949 0.0241 10 7 8 -0.1881 -0.0236 10 7 9 -0.2346 -0.0460 10 7 10 -0.1097 0.0134 10 7 11 0.1226 0.0519 10 7 12 0.0723 0.0028 10 7 13 -0.1685 -0.0307 10 8 0 -0.2215 -0.0266 10 8 1 0.4052 -0.0557 10 8 2 0.7760 -0.0343 10 8 3 0.0613 -0.0076 10 8 4 -0.8115 0.0076 10 8 5 -0.7728 0.0005 10 8 6 -0.2467 -0.0391 10 8 7 0.0591 -0.0423 10 8 8 0.1757 0.0293 10 8 9 0.1783 0.0573 10 8 10 -0.0089 -0.0179 10 8 11 -0.1726 -0.0622 10 8 12 -0.1075 -0.0144 10 9 0 -0.0511 0.0101 10 9 1 -0.5651 0.0684 10 9 2 -0.5963 0.0582 10 9 3 0.2297 0.0055 10 9 4 1.0126 -0.0376 10 9 5 1.0159 -0.0129 10 9 6 0.5805 0.0635 10 9 7 0.1804 0.0611 10 9 8 -0.0902 -0.0413 10 9 9 -0.1525 -0.0704 10 9 10 -0.0090 0.0192 10 9 11 0.1268 0.0613 10 9 12 0.1331 0.0164 10 10 0 0.1866 0.0066 10 10 1 0.4982 -0.0768 10 10 2 0.3371 -0.0736 10 10 3 -0.4318 0.0048 10 10 4 -1.1322 0.0681 10 10 5 -1.2329 0.0180 10 10 6 -0.8713 -0.0906 10 10 7 -0.3645 -0.0735 10 10 8 0.0626 0.0578 10 10 9 0.2417 0.0826 10 10 10 0.1642 -0.0169 10 10 11 -0.0168 -0.0516 10 11 0 -0.1856 -0.0200 10 11 1 -0.3000 0.0777 10 11 2 -0.0650 0.0802 10 11 3 0.5763 -0.0148 10 11 4 1.1701 -0.0893 10 11 5 1.2918 -0.0177 10 11 6 0.9429 0.1107 10 11 7 0.3774 0.0760 10 11 8 -0.1388 -0.0746 10 11 9 -0.4180 -0.0914 10 12 3 -0.6577 0.0193 10 12 4 -1.0458 0.0994 10 12 5 -1.0704 0.0169 10 12 6 -0.7401 -0.1175 10 12 7 -0.2409 -0.0690 11 -3 2 0.2409 0.0841 11 -3 3 -0.0650 0.1132 11 -3 4 -0.8776 0.0123 11 -3 5 -1.0366 -0.0976 11 -3 6 -0.0134 -0.0734 11 -3 7 0.8927 0.0096 11 -3 8 0.4431 -0.0129 11 -2 0 0.0162 0.0959 11 -2 1 -0.1310 -0.0067 11 -2 2 -0.0817 -0.0821 11 -2 3 0.6058 -0.0390 11 -2 4 1.2620 0.0506 11 -2 5 0.7460 0.0746 11 -2 6 -0.6328 0.0249 11 -2 7 -1.1160 0.0115 11 -2 8 -0.0708 0.0726 11 -2 9 0.9663 0.0939 11 -2 10 0.6879 0.0396 11 -1 0 0.1097 -0.0678 11 -1 1 0.0340 0.0204 11 -1 2 -0.2382 0.0358 11 -1 3 -0.9253 -0.0289 11 -1 4 -1.1575 -0.0586 11 -1 5 -0.1711 -0.0203 11 -1 6 1.0587 0.0047 11 -1 7 0.8915 -0.0444 11 -1 8 -0.4584 -0.1000 11 -1 9 -1.1354 -0.0626 11 -1 10 -0.3988 0.0119 11 -1 11 0.5868 0.0043 11 0 0 0.0221 0.0365 11 0 1 0.2254 -0.0057 11 0 2 0.3994 0.0174 11 0 3 0.7969 0.0527 11 0 4 0.6714 0.0211 11 0 5 -0.3347 -0.0272 11 0 6 -1.0166 -0.0053 11 0 7 -0.3079 0.0677 11 0 8 0.8699 0.0886 11 0 9 0.9214 0.0171 11 0 10 -0.0814 -0.0480 11 0 11 -0.8134 -0.0178 11 0 12 -0.7048 0.0334 11 1 0 -0.3250 -0.0180 11 1 1 -0.3787 -0.0198 11 1 2 -0.2055 -0.0436 11 1 3 -0.3212 -0.0316 11 1 4 -0.1426 0.0239 11 1 5 0.4958 0.0412 11 1 6 0.5480 -0.0120 11 1 7 -0.3439 -0.0669 11 1 8 -0.9525 -0.0534 11 1 9 -0.4026 0.0158 11 1 10 0.5254 0.0583 11 1 11 0.8123 0.0208 11 1 12 0.5515 -0.0420 11 2 0 0.5741 0.0148 11 2 1 0.2390 0.0332 11 2 2 -0.2482 0.0344 11 2 3 -0.1609 -0.0041 11 2 4 -0.1282 -0.0419 11 2 5 -0.3076 -0.0233 11 2 6 0.0623 0.0259 11 2 7 0.7747 0.0429 11 2 8 0.7038 0.0179 11 2 9 -0.1667 -0.0230 11 2 10 -0.7222 -0.0481 11 2 11 -0.5859 -0.0200 11 3 0 -0.5841 -0.0173 11 3 1 0.1418 -0.0241 11 3 2 0.6449 -0.0074 11 3 3 0.3350 0.0222 11 3 4 0.0900 0.0264 11 3 5 0.0067 -0.0030 11 3 6 -0.5003 -0.0214 11 3 7 -0.8786 -0.0091 11 3 8 -0.3201 0.0019 11 3 9 0.5153 0.0090 11 3 10 0.6028 0.0304 11 3 11 0.2446 0.0220 11 3 12 0.1877 -0.0488 11 4 0 0.3449 0.0147 11 4 1 -0.5141 -0.0009 11 4 2 -0.6905 -0.0138 11 4 3 -0.1361 -0.0129 11 4 4 0.0686 0.0024 11 4 5 0.1383 0.0135 11 4 6 0.6223 -0.0007 11 4 7 0.7539 -0.0196 11 4 8 0.0417 -0.0050 11 4 9 -0.5223 0.0124 11 4 10 -0.2717 -0.0149 11 4 11 0.0637 -0.0287 11 4 12 -0.0591 0.0351 11 4 13 -0.0875 0.0930 11 5 0 -0.0154 -0.0044 11 5 1 0.6242 0.0268 11 5 2 0.3271 0.0195 11 5 3 -0.2440 -0.0082 11 5 4 -0.1134 -0.0189 11 5 5 -0.0242 -0.0022 11 5 6 -0.4909 0.0273 11 5 7 -0.5704 0.0363 11 5 8 0.0170 0.0001 11 5 9 0.2728 -0.0308 11 5 10 -0.0730 0.0035 11 5 11 -0.2360 0.0383 11 5 12 -0.0307 -0.0115 11 6 0 -0.2064 -0.0073 11 6 1 -0.3977 -0.0433 11 6 2 0.2478 -0.0179 11 6 3 0.5394 0.0187 11 6 4 -0.0424 0.0143 11 6 5 -0.2569 -0.0174 11 6 6 0.2519 -0.0453 11 6 7 0.4173 -0.0444 11 6 8 0.0775 0.0032 11 6 9 0.0262 0.0443 11 6 10 0.2676 0.0067 11 6 11 0.2586 -0.0471 11 6 12 0.0872 -0.0142 11 7 0 0.2218 0.0119 11 7 1 -0.0264 0.0507 11 7 2 -0.7427 0.0235 11 7 3 -0.6084 -0.0092 11 7 4 0.3051 -0.0008 11 7 5 0.5457 0.0260 11 7 6 0.0086 0.0507 11 7 7 -0.2619 0.0523 11 7 8 -0.1654 -0.0021 11 7 9 -0.1968 -0.0564 11 7 10 -0.2724 -0.0178 11 7 11 -0.1936 0.0523 11 7 12 -0.1103 0.0336 11 8 0 -0.0777 -0.0061 11 8 1 0.4142 -0.0552 11 8 2 0.9676 -0.0420 11 8 3 0.4896 -0.0111 11 8 4 -0.5237 -0.0023 11 8 5 -0.7580 -0.0143 11 8 6 -0.2945 -0.0496 11 8 7 0.0357 -0.0657 11 8 8 0.1364 -0.0008 11 8 9 0.1936 0.0701 11 8 10 0.1685 0.0288 11 8 11 0.1297 -0.0522 11 9 0 -0.0956 -0.0067 11 9 1 -0.5951 0.0608 11 9 2 -0.9115 0.0660 11 9 3 -0.3075 0.0256 11 9 4 0.6266 -0.0148 11 9 5 0.9097 -0.0123 11 9 6 0.6154 0.0506 11 9 7 0.2541 0.0841 11 9 8 -0.0049 0.0017 11 9 9 -0.0967 -0.0839 11 9 10 -0.0814 -0.0369 11 10 2 0.6826 -0.0828 11 10 3 0.1462 -0.0252 11 10 4 -0.6468 0.0460 11 10 5 -1.0276 0.0406 11 10 6 -0.8999 -0.0577 11 10 7 -0.5031 -0.1026 11 10 8 -0.1302 0.0010 11 10 9 0.0219 0.0941 11 11 5 1.0659 -0.0599 12 -1 4 -1.2794 -0.0593 12 -1 5 -0.7827 -0.0343 12 -1 6 0.5818 0.0166 12 -1 7 1.1064 -0.0013 12 0 2 0.2434 0.0013 12 0 3 0.7446 0.0553 12 0 4 1.0346 0.0541 12 0 5 0.2831 -0.0157 12 0 6 -0.8694 -0.0456 12 0 7 -0.8497 0.0182 12 0 8 0.3271 0.0908 12 0 9 0.9526 0.0657 12 1 2 -0.3100 -0.0383 12 1 3 -0.4999 -0.0609 12 1 4 -0.5420 -0.0139 12 1 5 0.1400 0.0519 12 1 6 0.7882 0.0405 12 1 7 0.2998 -0.0359 12 1 8 -0.7225 -0.0779 12 1 9 -0.8041 -0.0302 12 1 10 0.0338 0.0462 12 2 1 0.3927 0.0283 12 2 2 0.1226 0.0466 12 2 3 0.1020 0.0313 12 2 4 0.1059 -0.0239 12 2 5 -0.3067 -0.0514 12 2 6 -0.4312 -0.0137 12 2 7 0.2726 0.0389 12 2 8 0.8676 0.0482 12 2 9 0.4487 0.0076 12 2 10 -0.3276 -0.0447 12 3 1 -0.2737 -0.0323 12 3 2 0.1663 -0.0268 12 3 3 0.1545 0.0034 12 3 4 0.0738 0.0313 12 3 5 0.2601 0.0212 12 3 6 0.0449 -0.0100 12 3 7 -0.6331 -0.0219 12 3 8 -0.7573 -0.0172 12 3 9 -0.0796 -0.0042 12 3 10 0.4181 0.0285 12 3 11 0.2667 0.0452 12 4 1 0.0149 0.0197 12 4 2 -0.3057 -0.0027 12 4 3 -0.0894 -0.0176 12 4 4 -0.0218 -0.0093 12 4 5 -0.1866 0.0116 12 4 6 0.1595 0.0117 12 4 7 0.7137 -0.0081 12 4 8 0.5307 -0.0052 12 4 9 -0.1178 0.0131 12 4 10 -0.2722 -0.0100 12 4 11 0.0163 -0.0465 12 5 1 0.1868 0.0022 12 5 2 0.1439 0.0231 12 5 3 -0.2423 0.0086 12 5 4 -0.0835 -0.0188 12 5 5 0.2367 -0.0228 12 5 6 -0.1342 0.0086 12 5 7 -0.6006 0.0387 12 5 8 -0.3460 0.0178 12 5 9 0.0844 -0.0241 12 5 10 -0.0086 -0.0053 12 5 11 -0.2564 0.0472 12 6 1 -0.1879 -0.0218 12 6 2 0.2583 -0.0294 12 6 3 0.6185 0.0062 12 6 4 0.0876 0.0297 12 6 5 -0.4097 0.0096 12 6 6 -0.0272 -0.0359 12 6 7 0.4175 -0.0606 12 6 8 0.2654 -0.0251 12 6 9 0.0906 0.0316 12 6 10 0.2577 0.0194 12 7 2 -0.6818 0.0304 12 7 3 -0.8302 -0.0083 12 7 4 0.0211 -0.0191 12 7 5 0.5896 0.0110 12 7 6 0.2110 0.0531 12 7 7 -0.2236 0.0721 12 7 8 -0.2399 0.0314 12 7 9 -0.2504 -0.0372 12 7 10 -0.3486 -0.0353 12 8 3 0.8167 -0.0066 12 8 4 -0.1400 0.0016 12 8 5 -0.6727 -0.0184 12 8 6 -0.3750 -0.0531 12 8 7 0.0115 -0.0775 12 8 8 0.1866 -0.0376 12 8 9 0.2835 0.0439 12 9 5 0.6539 0.0039 12 9 6 0.5350 0.0406 0 0 0 0.0 0.0 ; _shelx_fab_checksum 14964 _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 0.23390(3) 0.98022(2) 0.32142(2) 0.01042(6) Uani 1 1 d . . . . . Mo02 Mo 0.49272(3) 0.90987(2) -0.10266(2) 0.01056(6) Uani 1 1 d . . . . . Mo03 Mo 0.55328(3) 0.77318(3) 0.20049(2) 0.01340(7) Uani 1 1 d . . . . . Mo04 Mo 0.81297(3) 0.83876(3) -0.04373(2) 0.01224(6) Uani 1 1 d . . . . . Zn1 Zn 0.19840(5) 0.97638(4) 0.62943(4) 0.01688(9) Uani 1 1 d . . . . . O6 O 0.5547(3) 0.8783(2) 0.03211(19) 0.0130(4) Uani 1 1 d . . . . . O4 O 0.7341(3) 0.9213(2) -0.16343(19) 0.0138(5) Uani 1 1 d D . . . . O13 O 0.2620(3) 0.9340(2) 0.4527(2) 0.0171(5) Uani 1 1 d . . . . . O1 O 0.5193(3) 1.0150(2) -0.23949(19) 0.0132(4) Uani 1 1 d . . . . . O8 O 0.7574(3) 0.8028(2) 0.1239(2) 0.0162(5) Uani 1 1 d . . . . . O11 O 0.3254(3) 0.8309(2) 0.2426(2) 0.0137(5) Uani 1 1 d . . . . . O3 O 0.2920(3) 0.9554(2) -0.0334(2) 0.0166(5) Uani 1 1 d . . . . . O12 O 0.0408(3) 0.9921(2) 0.3521(2) 0.0188(5) Uani 1 1 d . . . . . O16 O 0.1843(3) 0.1652(2) 0.5610(2) 0.0253(6) Uani 1 1 d . . . . . O7 O 0.9862(3) 0.8740(2) -0.0716(2) 0.0223(5) Uani 1 1 d . . . . . O15 O 0.1200(3) 1.0510(2) 0.7925(2) 0.0223(5) Uani 1 1 d . . . . . H15 H 0.096572 0.995208 0.846123 0.034 Uiso 1 1 d R U . . . O5 O 0.8627(3) 0.6911(2) -0.0907(2) 0.0256(6) Uani 1 1 d . . . . . O10 O 0.5582(3) 0.7390(2) 0.3379(2) 0.0256(6) Uani 1 1 d . . . . . O14 O 0.4316(3) 0.9449(3) 0.6051(2) 0.0320(7) Uani 1 1 d . . . . . H14A H 0.472621 0.969367 0.645868 0.048 Uiso 1 1 d R U . . . H14B H 0.451591 0.908234 0.554704 0.048 Uiso 1 1 d R U . . . O9 O 0.5746(3) 0.6344(2) 0.1453(2) 0.0263(6) Uani 1 1 d . . . . . O2 O 0.5258(3) 0.7659(2) -0.1534(2) 0.0208(5) Uani 1 1 d . . . . . N3 N 0.2122(4) 0.5820(3) 0.2016(3) 0.0193(6) Uani 1 1 d . . . . . N2 N 0.2328(4) 0.6101(3) 0.5853(3) 0.0192(6) Uani 1 1 d . . . . . N1 N 0.2159(4) 0.7853(3) 0.6620(3) 0.0208(6) Uani 1 1 d . . . . . C8 C 0.1947(4) 0.2135(3) 0.4634(3) 0.0150(6) Uani 1 1 d . . . . . C10 C 0.2097(4) 0.5249(3) 0.3127(3) 0.0172(7) Uani 1 1 d . . . . . C6 C 0.2237(4) 0.5923(3) 0.3948(3) 0.0192(7) Uani 1 1 d . . . . . H6 H 0.234973 0.673106 0.377912 0.023 Uiso 1 1 calc R U . . . N4 N 0.1671(5) 0.7172(3) 0.0704(3) 0.0360(9) Uani 1 1 d . . . . . C7 C 0.2013(4) 0.3478(3) 0.4424(3) 0.0148(6) Uani 1 1 d . . . . . C12 C 0.1378(5) 0.6988(3) 0.1845(4) 0.0264(8) Uani 1 1 d . . . . . H12 H 0.076081 0.757161 0.242814 0.032 Uiso 1 1 calc R U . . . C9 C 0.1978(4) 0.4035(3) 0.3357(3) 0.0168(7) Uani 1 1 d . . . . . H9 H 0.187478 0.359503 0.280353 0.020 Uiso 1 1 calc R U . . . C5 C 0.2106(4) 0.4141(3) 0.5282(3) 0.0174(7) Uani 1 1 d . . . . . H5 H 0.210098 0.377394 0.600288 0.021 Uiso 1 1 calc R U . . . C1 C 0.1636(4) 0.7330(3) 0.5995(3) 0.0207(7) Uani 1 1 d . . . . . H1 H 0.088147 0.775635 0.568844 0.025 Uiso 1 1 calc R U . . . C4 C 0.2205(4) 0.5364(3) 0.5027(3) 0.0169(7) Uani 1 1 d . . . . . C11 C 0.2904(5) 0.5239(4) 0.0940(3) 0.0291(9) Uani 1 1 d . . . . . H11 H 0.350953 0.442351 0.080590 0.035 Uiso 1 1 calc R U . . . C13 C 0.2616(6) 0.6086(4) 0.0127(4) 0.0387(11) Uani 1 1 d . . . . . H13 H 0.298775 0.596261 -0.067928 0.046 Uiso 1 1 calc R U . . . C2 C 0.3242(5) 0.6903(3) 0.6898(3) 0.0273(9) Uani 1 1 d . . . . . H2 H 0.381418 0.699336 0.733609 0.033 Uiso 1 1 calc R U . . . C3 C 0.3354(5) 0.5818(3) 0.6441(4) 0.0289(9) Uani 1 1 d . . . . . H3 H 0.399389 0.504038 0.650991 0.035 Uiso 1 1 calc R U . . . O17 O 0.1995(3) 0.1632(2) 0.3730(2) 0.0180(5) Uani 1 1 d D . . . . 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 0.01296(13) 0.01071(13) 0.00881(12) 0.00059(10) -0.00400(10) -0.00504(10) Mo02 0.01361(13) 0.01078(13) 0.00972(12) 0.00131(10) -0.00582(11) -0.00518(10) Mo03 0.01539(14) 0.01112(13) 0.01312(13) 0.00274(10) -0.00529(11) -0.00337(10) Mo04 0.01257(14) 0.01352(13) 0.01128(13) 0.00193(10) -0.00569(11) -0.00316(10) Zn1 0.0211(2) 0.01607(19) 0.0170(2) -0.00205(15) -0.00881(17) -0.00671(16) O6 0.0142(11) 0.0152(11) 0.0106(10) 0.0027(9) -0.0055(9) -0.0051(9) O4 0.0151(11) 0.0167(11) 0.0109(11) 0.0038(9) -0.0062(9) -0.0054(9) O13 0.0238(13) 0.0161(11) 0.0119(11) 0.0002(9) -0.0062(10) -0.0063(10) O1 0.0163(12) 0.0164(11) 0.0103(10) 0.0025(9) -0.0078(9) -0.0063(9) O8 0.0169(12) 0.0193(12) 0.0150(11) 0.0045(9) -0.0089(10) -0.0060(10) O11 0.0137(11) 0.0141(11) 0.0149(11) -0.0003(9) -0.0054(9) -0.0057(9) O3 0.0164(12) 0.0177(12) 0.0172(12) -0.0002(9) -0.0062(10) -0.0065(10) O12 0.0159(12) 0.0208(12) 0.0214(13) -0.0022(10) -0.0064(10) -0.0070(10) O16 0.0504(18) 0.0146(12) 0.0163(12) 0.0025(10) -0.0141(13) -0.0145(12) O7 0.0173(13) 0.0257(13) 0.0240(13) 0.0047(11) -0.0072(11) -0.0079(10) O15 0.0338(15) 0.0219(13) 0.0168(12) 0.0044(10) -0.0116(12) -0.0139(11) O5 0.0314(15) 0.0165(12) 0.0275(14) -0.0024(11) -0.0107(12) -0.0028(11) O10 0.0279(15) 0.0286(14) 0.0203(13) 0.0062(11) -0.0116(12) -0.0054(11) O14 0.0340(16) 0.0510(19) 0.0239(15) -0.0043(13) -0.0171(13) -0.0198(14) O9 0.0304(15) 0.0150(12) 0.0304(15) -0.0035(11) -0.0067(12) -0.0053(11) O2 0.0243(14) 0.0163(12) 0.0226(13) -0.0018(10) -0.0077(11) -0.0067(10) N3 0.0283(17) 0.0159(14) 0.0173(15) 0.0054(12) -0.0116(13) -0.0086(12) N2 0.0285(17) 0.0120(13) 0.0208(15) -0.0005(11) -0.0119(13) -0.0066(12) N1 0.0260(17) 0.0189(15) 0.0212(15) -0.0022(12) -0.0094(13) -0.0095(13) C8 0.0179(17) 0.0162(16) 0.0144(15) -0.0004(13) -0.0068(13) -0.0084(13) C10 0.0210(17) 0.0146(16) 0.0170(16) 0.0022(13) -0.0088(14) -0.0041(13) C6 0.0269(19) 0.0105(15) 0.0228(18) 0.0022(13) -0.0103(15) -0.0080(14) N4 0.048(2) 0.0332(19) 0.035(2) 0.0130(16) -0.0242(19) -0.0150(17) C7 0.0183(17) 0.0099(15) 0.0166(16) -0.0010(12) -0.0061(14) -0.0040(12) C12 0.033(2) 0.0181(18) 0.032(2) 0.0060(16) -0.0183(19) -0.0060(16) C9 0.0218(18) 0.0135(16) 0.0182(17) -0.0006(13) -0.0083(14) -0.0076(13) C5 0.0226(18) 0.0150(16) 0.0157(16) 0.0017(13) -0.0080(14) -0.0056(13) C1 0.0218(18) 0.0147(16) 0.030(2) -0.0024(14) -0.0125(16) -0.0052(14) C4 0.0203(18) 0.0119(15) 0.0212(17) -0.0015(13) -0.0097(15) -0.0046(13) C11 0.040(2) 0.025(2) 0.0195(19) 0.0003(15) -0.0081(18) -0.0080(17) C13 0.053(3) 0.046(3) 0.0173(19) 0.0065(18) -0.010(2) -0.019(2) C2 0.043(2) 0.0236(19) 0.028(2) 0.0037(16) -0.0242(19) -0.0131(17) C3 0.043(2) 0.0178(18) 0.035(2) 0.0064(16) -0.027(2) -0.0068(17) O17 0.0328(15) 0.0109(11) 0.0142(11) -0.0008(9) -0.0107(11) -0.0082(10) 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' 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' Zn Zn 0.2839 1.4301 '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 O4 Mo01 O1 70.99(8) 2_675 2_675 ? O4 Mo01 O17 77.72(9) 2_675 1_565 ? O13 Mo01 O4 155.17(10) . 2_675 ? O13 Mo01 O1 89.26(10) . 2_675 ? O13 Mo01 O11 99.54(10) . . ? O13 Mo01 O17 85.60(10) . 1_565 ? O11 Mo01 O4 90.92(9) . 2_675 ? O11 Mo01 O1 77.51(9) . 2_675 ? O11 Mo01 O17 160.77(10) . 1_565 ? O12 Mo01 O4 95.01(10) . 2_675 ? O12 Mo01 O13 104.80(11) . . ? O12 Mo01 O1 165.84(10) . 2_675 ? O12 Mo01 O11 101.27(10) . . ? O12 Mo01 O17 95.20(10) . 1_565 ? O17 Mo01 O1 84.09(9) 1_565 2_675 ? O6 Mo02 O6 76.84(9) . 2_675 ? O6 Mo02 O4 73.22(9) . . ? O4 Mo02 O6 81.61(8) . 2_675 ? O1 Mo02 O6 74.57(8) . 2_675 ? O1 Mo02 O6 139.38(9) . . ? O1 Mo02 O4 74.57(9) . . ? O3 Mo02 O6 76.60(9) . 2_675 ? O3 Mo02 O6 100.15(10) . . ? O3 Mo02 O4 158.16(9) . . ? O3 Mo02 O1 100.59(10) . . ? O2 Mo02 O6 178.99(10) . 2_675 ? O2 Mo02 O6 104.05(11) . . ? O2 Mo02 O4 98.16(10) . . ? O2 Mo02 O1 104.41(11) . . ? O2 Mo02 O3 103.66(11) . . ? O6 Mo03 O1 72.14(8) . 2_675 ? O8 Mo03 O6 72.95(9) . . ? O8 Mo03 O1 83.05(9) . 2_675 ? O8 Mo03 O11 149.96(9) . . ? O11 Mo03 O6 82.94(9) . . ? O11 Mo03 O1 72.51(8) . 2_675 ? O10 Mo03 O6 161.13(11) . . ? O10 Mo03 O1 90.27(10) . 2_675 ? O10 Mo03 O8 98.75(11) . . ? O10 Mo03 O11 98.55(11) . . ? O9 Mo03 O6 93.70(11) . . ? O9 Mo03 O1 162.63(11) . 2_675 ? O9 Mo03 O8 102.77(12) . . ? O9 Mo03 O11 96.29(11) . . ? O9 Mo03 O10 104.78(13) . . ? O6 Mo04 O3 70.71(8) . 2_675 ? O4 Mo04 O6 72.24(9) . . ? O4 Mo04 O8 144.16(10) . . ? O4 Mo04 O3 80.57(9) . 2_675 ? O8 Mo04 O6 73.26(9) . . ? O8 Mo04 O3 79.22(9) . 2_675 ? O7 Mo04 O6 153.26(10) . . ? O7 Mo04 O4 107.00(11) . . ? O7 Mo04 O8 99.42(11) . . ? O7 Mo04 O3 82.71(10) . 2_675 ? O5 Mo04 O6 101.64(11) . . ? O5 Mo04 O4 97.98(11) . . ? O5 Mo04 O8 98.13(11) . . ? O5 Mo04 O3 172.32(11) . 2_675 ? O5 Mo04 O7 104.88(13) . . ? O13 Zn1 O12 88.71(9) . 2_576 ? O13 Zn1 O16 83.00(9) . 1_565 ? O13 Zn1 N1 85.74(10) . . ? O12 Zn1 O16 87.17(10) 2_576 1_565 ? O15 Zn1 O13 169.21(10) . . ? O15 Zn1 O12 87.35(10) . 2_576 ? O15 Zn1 O16 86.77(10) . 1_565 ? O15 Zn1 O14 94.69(11) . . ? O15 Zn1 N1 104.32(11) . . ? O14 Zn1 O13 89.20(10) . . ? O14 Zn1 O12 177.90(10) . 2_576 ? O14 Zn1 O16 92.44(11) . 1_565 ? O14 Zn1 N1 89.55(12) . . ? N1 Zn1 O12 90.44(11) . 2_576 ? N1 Zn1 O16 168.54(10) . 1_565 ? Mo02 O6 Mo02 103.16(9) . 2_675 ? Mo02 O6 Mo03 150.49(12) . . ? Mo02 O6 Mo04 104.25(10) . . ? Mo03 O6 Mo02 97.83(8) . 2_675 ? Mo04 O6 Mo02 96.57(8) . 2_675 ? Mo04 O6 Mo03 93.57(8) . . ? Mo01 O4 Mo02 104.48(9) 2_675 . ? Mo04 O4 Mo01 149.89(13) . 2_675 ? Mo04 O4 Mo02 105.61(10) . . ? Mo01 O13 Zn1 146.38(14) . . ? Mo01 O1 Mo03 90.50(8) 2_675 2_675 ? Mo02 O1 Mo01 109.42(10) . 2_675 ? Mo02 O1 Mo03 114.29(10) . 2_675 ? Mo03 O8 Mo04 114.65(11) . . ? Mo01 O11 Mo03 114.91(11) . . ? Mo02 O3 Mo04 116.03(11) . 2_675 ? Mo01 O12 Zn1 172.34(15) . 2_576 ? C8 O16 Zn1 133.9(2) . 1_545 ? Zn1 O15 H15 110.3 . . ? Zn1 O14 H14A 129.2 . . ? Zn1 O14 H14B 89.6 . . ? H14A O14 H14B 141.3 . . ? C12 N3 C10 126.0(3) . . ? C12 N3 C11 108.8(3) . . ? C11 N3 C10 125.2(3) . . ? C1 N2 C4 123.0(3) . . ? C1 N2 C3 106.8(3) . . ? C3 N2 C4 128.8(3) . . ? C1 N1 Zn1 115.0(2) . . ? C1 N1 C2 105.2(3) . . ? C2 N1 Zn1 132.6(2) . . ? O16 C8 C7 119.4(3) . . ? O16 C8 O17 127.6(3) . . ? O17 C8 C7 112.9(3) . . ? C6 C10 N3 118.9(3) . . ? C9 C10 N3 120.0(3) . . ? C9 C10 C6 121.1(3) . . ? C10 C6 H6 120.7 . . ? C10 C6 C4 118.6(3) . . ? C4 C6 H6 120.7 . . ? C12 N4 C13 108.7(3) . . ? C9 C7 C8 118.3(3) . . ? C9 C7 C5 121.1(3) . . ? C5 C7 C8 120.7(3) . . ? N3 C12 H12 125.8 . . ? N4 C12 N3 108.3(4) . . ? N4 C12 H12 125.8 . . ? C10 C9 C7 119.3(3) . . ? C10 C9 H9 120.4 . . ? C7 C9 H9 120.4 . . ? C7 C5 H5 121.0 . . ? C4 C5 C7 118.1(3) . . ? C4 C5 H5 121.0 . . ? N2 C1 H1 124.1 . . ? N1 C1 N2 111.8(3) . . ? N1 C1 H1 124.1 . . ? C6 C4 N2 116.7(3) . . ? C5 C4 N2 121.5(3) . . ? C5 C4 C6 121.8(3) . . ? N3 C11 H11 126.8 . . ? C13 C11 N3 106.5(4) . . ? C13 C11 H11 126.8 . . ? N4 C13 H13 126.1 . . ? C11 C13 N4 107.7(4) . . ? C11 C13 H13 126.1 . . ? N1 C2 H2 124.9 . . ? C3 C2 N1 110.2(3) . . ? C3 C2 H2 124.9 . . ? N2 C3 H3 127.0 . . ? C2 C3 N2 105.9(3) . . ? C2 C3 H3 127.0 . . ? C8 O17 Mo01 136.0(2) . 1_545 ? 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 O4 2.077(2) 2_675 ? Mo01 O13 1.728(2) . ? Mo01 O1 2.221(2) 2_675 ? Mo01 O11 1.848(2) . ? Mo01 O12 1.722(2) . ? Mo01 O17 2.111(2) 1_565 ? Mo02 O6 2.477(2) 2_675 ? Mo02 O6 1.922(2) . ? Mo02 O4 2.196(2) . ? Mo02 O1 1.912(2) . ? Mo02 O3 1.744(2) . ? Mo02 O2 1.696(2) . ? Mo03 O6 2.252(2) . ? Mo03 O1 2.327(2) 2_675 ? Mo03 O8 1.940(2) . ? Mo03 O11 1.984(2) . ? Mo03 O10 1.699(2) . ? Mo03 O9 1.693(2) . ? Mo04 O6 2.235(2) . ? Mo04 O4 1.925(2) . ? Mo04 O8 1.945(2) . ? Mo04 O3 2.388(2) 2_675 ? Mo04 O7 1.720(2) . ? Mo04 O5 1.690(2) . ? Zn1 O13 2.093(2) . ? Zn1 O12 2.156(2) 2_576 ? Zn1 O16 2.166(2) 1_565 ? Zn1 O15 2.043(2) . ? Zn1 O14 2.081(3) . ? Zn1 N1 2.098(3) . ? O16 C8 1.236(4) . ? O15 H15 0.8639 . ? O14 H14A 0.8480 . ? O14 H14B 0.7152 . ? N3 C10 1.431(4) . ? N3 C12 1.338(4) . ? N3 C11 1.384(5) . ? N2 C1 1.349(4) . ? N2 C4 1.433(4) . ? N2 C3 1.377(5) . ? N1 C1 1.317(4) . ? N1 C2 1.376(5) . ? C8 C7 1.508(4) . ? C8 O17 1.279(4) . ? C10 C6 1.389(5) . ? C10 C9 1.381(4) . ? C6 H6 0.9300 . ? C6 C4 1.389(5) . ? N4 C12 1.324(5) . ? N4 C13 1.380(6) . ? C7 C9 1.392(5) . ? C7 C5 1.395(5) . ? C12 H12 0.9300 . ? C9 H9 0.9300 . ? C5 H5 0.9300 . ? C5 C4 1.389(5) . ? C1 H1 0.9300 . ? C11 H11 0.9300 . ? C11 C13 1.346(6) . ? C13 H13 0.9300 . ? C2 H2 0.9300 . ? C2 C3 1.354(5) . ? C3 H3 0.9300 . ? 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_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Zn1 O16 C8 C7 -171.3(2) 1_545 . . . ? Zn1 O16 C8 O17 9.5(6) 1_545 . . . ? Zn1 N1 C1 N2 153.9(2) . . . . ? Zn1 N1 C2 C3 -147.8(3) . . . . ? O6 Mo02 O3 Mo04 76.15(12) . . . 2_675 ? O6 Mo02 O3 Mo04 2.44(9) 2_675 . . 2_675 ? O4 Mo01 O13 Zn1 82.6(4) 2_675 . . . ? O4 Mo01 O11 Mo03 89.25(12) 2_675 . . . ? O4 Mo02 O3 Mo04 6.1(3) . . . 2_675 ? O13 Mo01 O11 Mo03 -68.13(13) . . . . ? O1 Mo01 O13 Zn1 119.1(2) 2_675 . . . ? O1 Mo01 O11 Mo03 18.96(10) 2_675 . . . ? O1 Mo02 O3 Mo04 -68.73(12) . . . 2_675 ? O11 Mo01 O13 Zn1 -163.7(2) . . . . ? O12 Mo01 O13 Zn1 -59.3(3) . . . . ? O12 Mo01 O11 Mo03 -175.45(12) . . . . ? O16 C8 C7 C9 -173.8(3) . . . . ? O16 C8 C7 C5 6.1(5) . . . . ? O16 C8 O17 Mo01 -13.6(6) . . . 1_545 ? O2 Mo02 O3 Mo04 -176.56(12) . . . 2_675 ? N3 C10 C6 C4 179.7(3) . . . . ? N3 C10 C9 C7 177.6(3) . . . . ? N3 C11 C13 N4 0.1(5) . . . . ? N1 C2 C3 N2 0.6(5) . . . . ? C8 C7 C9 C10 -177.5(3) . . . . ? C8 C7 C5 C4 178.3(3) . . . . ? C10 N3 C12 N4 -179.5(3) . . . . ? C10 N3 C11 C13 179.2(3) . . . . ? C10 C6 C4 N2 -179.0(3) . . . . ? C10 C6 C4 C5 2.9(5) . . . . ? C6 C10 C9 C7 -0.6(5) . . . . ? C7 C8 O17 Mo01 167.1(2) . . . 1_545 ? C7 C5 C4 N2 -179.0(3) . . . . ? C7 C5 C4 C6 -1.0(5) . . . . ? C12 N3 C10 C6 -43.4(5) . . . . ? C12 N3 C10 C9 138.4(4) . . . . ? C12 N3 C11 C13 0.3(5) . . . . ? C12 N4 C13 C11 -0.5(5) . . . . ? C9 C10 C6 C4 -2.1(5) . . . . ? C9 C7 C5 C4 -1.7(5) . . . . ? C5 C7 C9 C10 2.5(5) . . . . ? C1 N2 C4 C6 38.7(5) . . . . ? C1 N2 C4 C5 -143.1(4) . . . . ? C1 N2 C3 C2 -0.8(4) . . . . ? C1 N1 C2 C3 -0.3(5) . . . . ? C4 N2 C1 N1 -167.3(3) . . . . ? C4 N2 C3 C2 166.2(4) . . . . ? C11 N3 C10 C6 137.9(4) . . . . ? C11 N3 C10 C9 -40.3(5) . . . . ? C11 N3 C12 N4 -0.6(4) . . . . ? C13 N4 C12 N3 0.7(5) . . . . ? C2 N1 C1 N2 -0.3(4) . . . . ? C3 N2 C1 N1 0.7(4) . . . . ? C3 N2 C4 C6 -126.4(4) . . . . ? C3 N2 C4 C5 51.7(5) . . . . ? O17 Mo01 O13 Zn1 35.0(2) 1_565 . . . ? O17 Mo01 O11 Mo03 36.1(3) 1_565 . . . ? O17 C8 C7 C9 5.5(5) . . . . ? O17 C8 C7 C5 -174.5(3) . . . . ? 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 0.000 0.500 1.000 46.0 9.3 ?