#------------------------------------------------------------------------------ #$Date: 2021-12-07 04:50:57 +0200 (Tue, 07 Dec 2021) $ #$Revision: 271153 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/37/7243749.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_7243749 loop_ _publ_author_name 'Ying, Jun' 'Jin, Liang' 'Yu, Hai-Yan' 'Tian, Ai-Xiang' 'Wang, Xiu-Li' _publ_section_title ; A series of polyoxometalate-based hybrid complexes constructed by a tripodal ligand containing mixed N/O donors ; _journal_issue 44 _journal_name_full CrystEngComm _journal_page_first 7846 _journal_page_last 7854 _journal_paper_doi 10.1039/D1CE01195B _journal_volume 23 _journal_year 2021 _chemical_formula_moiety 'C13 H13 Mo4 N4 Ni O17' _chemical_formula_sum 'C13 H13 Mo4 N4 Ni O17' _chemical_formula_weight 939.74 _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.cc26rrqg _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 83.6190(10) _cell_angle_beta 68.1620(10) _cell_angle_gamma 74.0840(10) _cell_formula_units_Z 2 _cell_length_a 9.5458(5) _cell_length_b 11.1569(6) _cell_length_c 12.2071(7) _cell_measurement_reflns_used 5088 _cell_measurement_temperature 273.15 _cell_measurement_theta_max 28.40 _cell_measurement_theta_min 2.38 _cell_volume 1160.46(11) _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 273.15 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.990 _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 0.0119 _diffrn_reflns_av_unetI/netI 0.0250 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 8513 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.397 _diffrn_reflns_theta_min 1.797 _diffrn_source_current 30.0 _diffrn_source_power 1.2 _diffrn_source_voltage 40.0 _exptl_absorpt_coefficient_mu 2.992 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6910 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0438 before and 0.0219 after correction. The Ratio of minimum to maximum transmission is 0.9266. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.689 _exptl_crystal_description block _exptl_crystal_F_000 902 _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.886 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.110 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 354 _refine_ls_number_reflns 5772 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.032 _refine_ls_R_factor_all 0.0270 _refine_ls_R_factor_gt 0.0219 _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^)+(0.0276P)^2^+0.8552P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.0541 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5143 _reflns_number_total 5772 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1ce01195b2.cif _cod_data_source_block 2_CCDC4 _cod_depositor_comments 'Adding full bibliography for 7243745--7243750.cif.' _cod_database_code 7243749 _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,H) groups 2.a Rotating group: O14(H14A,H14B), O15(H15A,H15B) 2.b Aromatic/amide H refined with riding coordinates: C5(H5), C2(H2), C9(H9), C8(H8), C13(H13), C11(H11), C3(H3), C1(H1), C12(H12) ; _shelx_res_file ; TITL 2_a.res in P-1 2.res created by SHELXL-2018/3 at 10:59:38 on 07-Dec-2020 REM Old TITL 2 in P-1 REM SHELXT solution in P-1 REM R1 0.050, Rweak 0.004, Alpha 0.037, Orientation as input REM Formula found by SHELXT: C14 N5 O15 Ni Mo4 CELL 0.71073 9.5458 11.1569 12.2071 83.619 68.162 74.084 ZERR 2 0.0005 0.0006 0.0007 0.001 0.001 0.001 LATT 1 SFAC C H Mo N Ni O UNIT 26 26 8 8 2 34 L.S. 10 0 0 PLAN 50 TEMP 0 CONF list 4 ABIN fmap 2 53 acta MORE -1 BOND $H REM REM REM WGHT 0.027600 0.855200 FVAR 0.33519 MO4 3 0.232342 0.979625 0.322078 11.00000 0.01277 0.01029 = 0.00736 -0.00019 -0.00256 -0.00401 MO2 3 0.491918 0.910699 -0.103340 11.00000 0.01396 0.01074 = 0.00857 0.00079 -0.00436 -0.00444 MO3 3 0.552789 0.771894 0.200415 11.00000 0.01557 0.01100 = 0.01163 0.00207 -0.00385 -0.00290 MO1 3 0.814240 0.837499 -0.044284 11.00000 0.01322 0.01351 = 0.00992 0.00141 -0.00432 -0.00270 NI1 5 0.195178 0.979578 0.625213 11.00000 0.01760 0.01223 = 0.01078 -0.00085 -0.00522 -0.00534 O4 6 0.735697 0.921831 -0.164658 11.00000 0.01699 0.01568 = 0.00846 0.00179 -0.00370 -0.00503 O6 6 0.553940 0.878356 0.032167 11.00000 0.01482 0.01650 = 0.00860 0.00329 -0.00446 -0.00450 O10 6 0.322452 0.830011 0.243218 11.00000 0.01617 0.01169 = 0.01416 -0.00102 -0.00515 -0.00504 O13 6 0.260051 0.933472 0.454311 11.00000 0.02146 0.01270 = 0.01066 -0.00075 -0.00525 -0.00296 O8 6 0.758314 0.801476 0.123890 11.00000 0.01558 0.01808 = 0.01417 0.00347 -0.00728 -0.00483 O17 6 0.198855 0.162222 0.375779 11.00000 0.03097 0.01149 = 0.01412 0.00000 -0.00949 -0.00675 O2 6 0.289939 0.956181 -0.034340 11.00000 0.01702 0.01825 = 0.01511 0.00059 -0.00491 -0.00586 O16 6 0.186787 0.164107 0.563919 11.00000 0.03988 0.01447 = 0.01297 0.00085 -0.00933 -0.01077 O12 6 0.037346 0.991631 0.353164 11.00000 0.01455 0.01611 = 0.01900 -0.00091 -0.00503 -0.00381 O1AA 6 0.989072 0.871560 -0.071138 11.00000 0.01728 0.02609 = 0.02007 0.00453 -0.00617 -0.00703 O14 6 0.425365 0.946304 0.604358 11.00000 0.02544 0.03750 = 0.01868 -0.00435 -0.00864 -0.01115 AFIX 7 H14A 2 0.509477 0.908894 0.539845 11.00000 -1.50000 H14B 2 0.435446 0.988103 0.655506 11.00000 -1.50000 AFIX 0 O15 6 0.120015 1.048330 0.790187 11.00000 0.03128 0.02237 = 0.01347 0.00176 -0.00898 -0.01261 AFIX 7 H15A 2 0.193048 1.072114 0.800589 11.00000 -1.50000 H15B 2 0.102768 0.989841 0.842447 11.00000 -1.50000 AFIX 0 O0AA 6 0.524595 0.766862 -0.154884 11.00000 0.02552 0.01567 = 0.02148 -0.00275 -0.00816 -0.00592 O11 6 0.556274 0.736875 0.338748 11.00000 0.02572 0.02848 = 0.01832 0.00640 -0.00886 -0.00321 O5 6 0.862687 0.690071 -0.092683 11.00000 0.03290 0.01737 = 0.02578 -0.00269 -0.01063 -0.00248 O9 6 0.572488 0.633561 0.144260 11.00000 0.02799 0.01692 = 0.02880 -0.00488 -0.00533 -0.00452 N2 4 0.209942 0.581320 0.203789 11.00000 0.02683 0.01437 = 0.01605 0.00397 -0.00798 -0.00690 N4 4 0.213087 0.790150 0.662241 11.00000 0.02659 0.01704 = 0.01478 -0.00004 -0.00775 -0.00969 N3 4 0.230601 0.612394 0.588835 11.00000 0.02730 0.01072 = 0.01991 -0.00132 -0.00947 -0.00655 C7 1 0.195934 0.212731 0.465853 11.00000 0.01609 0.01070 = 0.01337 -0.00169 -0.00317 -0.00399 N1 4 0.162969 0.716786 0.073450 11.00000 0.04934 0.03070 = 0.02909 0.01245 -0.02225 -0.01138 C4 1 0.208555 0.524610 0.315589 11.00000 0.02242 0.01465 = 0.01370 0.00212 -0.00647 -0.00530 C6 1 0.201692 0.347285 0.444915 11.00000 0.01782 0.01082 = 0.01414 -0.00032 -0.00279 -0.00410 C5 1 0.198158 0.402552 0.337531 11.00000 0.02174 0.01383 = 0.01643 0.00044 -0.00742 -0.00643 AFIX 43 H5 2 0.188957 0.358042 0.281572 11.00000 -1.20000 AFIX 0 C2 1 0.133921 0.698251 0.187686 11.00000 0.03662 0.01931 = 0.02772 0.00650 -0.01749 -0.00716 AFIX 43 H2 2 0.071577 0.756226 0.246692 11.00000 -1.20000 AFIX 0 C9 1 0.222274 0.592862 0.397721 11.00000 0.02639 0.01108 = 0.01995 0.00200 -0.00996 -0.00599 AFIX 43 H9 2 0.233155 0.673883 0.380619 11.00000 -1.20000 AFIX 0 C8 1 0.211674 0.414516 0.530979 11.00000 0.02264 0.01348 = 0.01462 0.00058 -0.00724 -0.00487 AFIX 43 H8 2 0.213077 0.377614 0.602853 11.00000 -1.20000 AFIX 0 C13 1 0.320450 0.697005 0.692694 11.00000 0.04180 0.02169 = 0.02529 0.00193 -0.02137 -0.00869 AFIX 43 H13 2 0.376318 0.708019 0.737411 11.00000 -1.20000 AFIX 0 C11 1 0.161591 0.735683 0.601084 11.00000 0.02481 0.01386 = 0.02406 -0.00199 -0.00996 -0.00520 AFIX 43 H11 2 0.086067 0.777056 0.569587 11.00000 -1.20000 AFIX 0 C10 1 0.219415 0.537544 0.506317 11.00000 0.02136 0.01220 = 0.01859 -0.00309 -0.00749 -0.00486 C3 1 0.288654 0.524437 0.095538 11.00000 0.03842 0.02361 = 0.01692 -0.00088 -0.00579 -0.00642 AFIX 43 H3 2 0.350161 0.443114 0.081452 11.00000 -1.20000 AFIX 0 C1 1 0.259570 0.608762 0.014488 11.00000 0.04947 0.04157 = 0.01800 0.00460 -0.01078 -0.01532 AFIX 43 H1 2 0.297447 0.596798 -0.066596 11.00000 -1.20000 AFIX 0 C12 1 0.333642 0.586106 0.648165 11.00000 0.04215 0.01652 = 0.03189 0.00408 -0.02434 -0.00566 AFIX 43 H12 2 0.398365 0.509043 0.656082 11.00000 -1.20000 AFIX 0 O7 6 0.480795 0.983865 0.240601 11.00000 0.01455 0.01558 = 0.01001 0.00220 -0.00503 -0.00517 HKLF 4 REM 2_a.res in P-1 REM wR2 = 0.0541, GooF = S = 1.032, Restrained GooF = 1.032 for all data REM R1 = 0.0219 for 5143 Fo > 4sig(Fo) and 0.0270 for all 5772 data REM 354 parameters refined using 0 restraints END WGHT 0.0275 0.8549 REM Highest difference peak 0.886, deepest hole -0.652, 1-sigma level 0.110 Q1 1 0.1377 0.9823 0.3182 11.00000 0.05 0.89 Q2 1 0.9045 0.8403 -0.0387 11.00000 0.05 0.86 Q3 1 0.3152 0.9790 0.3197 11.00000 0.05 0.74 Q4 1 0.1238 0.7873 0.0381 11.00000 0.05 0.69 Q5 1 0.3927 0.9172 -0.1085 11.00000 0.05 0.66 Q6 1 0.7312 0.8220 -0.0456 11.00000 0.05 0.64 Q7 1 0.6427 0.7751 0.1919 11.00000 0.05 0.60 Q8 1 0.6247 0.7541 0.2422 11.00000 0.05 0.59 Q9 1 0.5865 0.9161 -0.1185 11.00000 0.05 0.55 Q10 1 0.4776 0.7844 0.1788 11.00000 0.05 0.54 Q11 1 0.2001 0.2801 0.4518 11.00000 0.05 0.48 Q12 1 0.1235 1.0041 0.5829 11.00000 0.05 0.47 Q13 1 0.2026 0.4613 0.3332 11.00000 0.05 0.44 Q14 1 0.2834 0.9991 0.6266 11.00000 0.05 0.44 Q15 1 0.6308 0.9401 -0.1219 11.00000 0.05 0.43 Q16 1 0.1656 0.6255 0.6255 11.00000 0.05 0.43 Q17 1 0.1410 0.6016 0.2035 11.00000 0.05 0.42 Q18 1 0.8796 0.9144 -0.0445 11.00000 0.05 0.42 Q19 1 0.2013 0.1032 0.3813 11.00000 0.05 0.41 Q20 1 0.2501 0.5563 0.1537 11.00000 0.05 0.41 Q21 1 0.2276 0.4784 0.5191 11.00000 0.05 0.40 Q22 1 0.4432 0.7685 0.2170 11.00000 0.05 0.39 Q23 1 0.1297 1.1387 0.8214 11.00000 0.05 0.39 Q24 1 0.5325 0.9019 -0.0280 11.00000 0.05 0.39 Q25 1 0.6842 0.8831 -0.0922 11.00000 0.05 0.38 Q26 1 0.5097 0.9004 0.0042 11.00000 0.05 0.38 Q27 1 0.2178 0.6426 0.1975 11.00000 0.05 0.38 Q28 1 0.2377 0.5579 0.4480 11.00000 0.05 0.38 Q29 1 0.4420 1.0174 0.1979 11.00000 0.05 0.38 Q30 1 0.2732 0.5869 0.6182 11.00000 0.05 0.37 Q31 1 0.4882 0.7567 0.3166 11.00000 0.05 0.36 Q32 1 0.1990 0.1853 0.6006 11.00000 0.05 0.36 Q33 1 0.2489 0.3841 0.4769 11.00000 0.05 0.36 Q34 1 0.2359 0.6582 0.5747 11.00000 0.05 0.36 Q35 1 0.5053 0.6797 0.1863 11.00000 0.05 0.35 Q36 1 0.1921 0.6629 0.0399 11.00000 0.05 0.35 Q37 1 0.4935 0.8616 0.6214 11.00000 0.05 0.35 Q38 1 0.2813 0.9384 0.6647 11.00000 0.05 0.34 Q39 1 1.0211 0.8534 -0.0917 11.00000 0.05 0.34 Q40 1 0.3563 0.9860 -0.0838 11.00000 0.05 0.34 Q41 1 0.1187 1.0764 0.6313 11.00000 0.05 0.34 Q42 1 0.6334 0.6103 0.1931 11.00000 0.05 0.34 Q43 1 0.7923 0.8405 0.0818 11.00000 0.05 0.33 Q44 1 0.4668 0.8045 -0.1115 11.00000 0.05 0.33 Q45 1 0.6008 0.7890 -0.1580 11.00000 0.05 0.33 Q46 1 0.7384 1.0012 -0.1328 11.00000 0.05 0.33 Q47 1 0.3679 1.0450 0.6092 11.00000 0.05 0.32 Q48 1 0.3968 0.9935 0.3414 11.00000 0.05 0.32 Q49 1 0.2495 0.7190 0.0657 11.00000 0.05 0.32 Q50 1 0.9566 0.9379 -0.0649 11.00000 0.05 0.32 ; _shelx_res_checksum 55331 _shelx_fab_file ; -11 -7 1 0.0832 0.0283 -11 -6 1 -0.1655 -0.0075 -11 -5 1 0.1838 -0.0021 -11 -5 2 -0.6700 0.0147 -11 -4 1 -0.0954 0.0074 -11 -4 2 0.8338 -0.0036 -11 -3 1 -0.0714 -0.0170 -11 -3 2 -0.8952 -0.0148 -11 -2 1 0.2298 0.0319 -11 -2 2 0.7904 0.0293 -11 -1 1 -0.2923 -0.0438 -11 -1 2 -0.5362 -0.0296 -11 0 1 0.2305 0.0420 -10 -10 1 -0.1976 -0.0682 -10 -9 1 0.1955 0.0715 -10 -7 1 0.3097 0.0331 -10 -7 2 -0.2173 0.0098 -10 -6 1 -0.4490 -0.0087 -10 -6 2 0.2838 -0.0025 -10 -5 1 0.5583 -0.0061 -10 -5 2 -0.4386 0.0009 -10 -5 3 -0.8824 0.0256 -10 -4 1 -0.5437 0.0127 -10 -4 2 0.6787 0.0049 -10 -4 3 1.0714 -0.0100 -10 -3 1 0.3664 -0.0197 -10 -3 2 -0.9165 -0.0193 -10 -3 3 -1.0692 -0.0122 -10 -2 1 -0.0796 0.0337 -10 -2 2 1.0238 0.0357 -10 -2 3 0.8207 0.0261 -10 -1 1 -0.1972 -0.0511 -10 -1 2 -0.9164 -0.0415 -10 -1 3 -0.3948 -0.0248 -10 -1 4 0.5918 0.0049 -10 0 1 0.3500 0.0604 -10 0 2 0.6153 0.0286 -10 0 3 -0.0431 0.0145 -10 0 4 -0.7189 0.0063 -10 1 1 -0.3364 -0.0518 -10 1 2 -0.2397 -0.0014 -10 1 3 0.3260 -0.0091 -10 2 1 0.1998 0.0282 -10 2 2 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1 0.8118 -0.0117 10 1 2 0.1563 -0.0237 10 1 3 -0.2393 -0.0057 10 1 4 -0.2315 0.0043 10 1 5 -0.2057 -0.0125 10 1 6 -0.2247 -0.0405 10 1 7 -0.1321 -0.0415 10 1 8 -0.0193 -0.0051 10 1 9 -0.1306 0.0257 10 1 10 -0.3869 0.0315 10 1 11 -0.3565 0.0464 10 1 12 0.0669 0.0622 10 1 13 0.3851 0.0341 10 2 0 -1.0633 -0.0083 10 2 1 -0.7842 0.0176 10 2 2 0.0839 0.0105 10 2 3 0.4707 -0.0118 10 2 4 0.3803 -0.0140 10 2 5 0.2618 0.0057 10 2 6 0.1589 0.0231 10 2 7 0.0113 0.0141 10 2 8 0.0053 -0.0122 10 2 9 0.2617 -0.0226 10 2 10 0.5003 -0.0210 10 2 11 0.3188 -0.0325 10 2 12 -0.1711 -0.0338 10 2 13 -0.3988 -0.0032 10 2 14 -0.2040 0.0227 10 3 0 1.1702 0.0012 10 3 1 0.6246 -0.0097 10 3 2 -0.3143 0.0041 10 3 3 -0.6310 0.0167 10 3 4 -0.4677 0.0130 10 3 5 -0.2603 0.0040 10 3 6 -0.0674 -0.0021 10 3 7 0.0546 0.0002 10 3 8 -0.0603 0.0071 10 3 9 -0.3434 0.0053 10 3 10 -0.4583 0.0027 10 3 11 -0.1845 0.0110 10 3 12 0.2304 0.0098 10 3 13 0.3196 -0.0079 10 3 14 0.0823 -0.0159 10 4 0 -1.0856 -0.0017 10 4 1 -0.4092 -0.0021 10 4 2 0.4480 -0.0132 10 4 3 0.6668 -0.0111 10 4 4 0.4689 -0.0069 10 4 5 0.2136 -0.0123 10 4 6 -0.0013 -0.0096 10 4 7 -0.0392 0.0014 10 4 8 0.1411 0.0067 10 4 9 0.3166 0.0106 10 4 10 0.2729 0.0115 10 4 11 0.0193 0.0016 10 4 12 -0.2170 -0.0042 10 4 13 -0.1826 0.0024 10 4 14 0.0346 0.0077 10 5 0 0.8744 0.0009 10 5 1 0.2353 0.0141 10 5 2 -0.4379 0.0201 10 5 3 -0.5813 0.0018 10 5 4 -0.4081 -0.0021 10 5 5 -0.1560 0.0137 10 5 6 0.0260 0.0113 10 5 7 -0.0299 -0.0059 10 5 8 -0.1947 -0.0130 10 5 9 -0.1833 -0.0155 10 5 10 -0.0177 -0.0130 10 5 11 0.1177 0.0043 10 5 12 0.1502 0.0152 10 5 13 0.0448 0.0045 10 5 14 -0.1168 -0.0073 10 6 0 -0.6431 0.0026 10 6 1 -0.1628 -0.0308 10 6 2 0.3064 -0.0301 10 6 3 0.4309 0.0074 10 6 4 0.3286 0.0138 10 6 5 0.1025 -0.0106 10 6 6 -0.0295 -0.0143 10 6 7 0.1033 -0.0008 10 6 8 0.2043 0.0063 10 6 9 0.0035 0.0098 10 6 10 -0.2229 -0.0002 10 6 11 -0.2064 -0.0255 10 6 12 -0.0769 -0.0277 10 6 13 0.0513 0.0005 10 7 0 0.4723 -0.0020 10 7 1 0.1812 0.0561 10 7 2 -0.1292 0.0430 10 7 3 -0.2828 -0.0164 10 7 4 -0.2516 -0.0244 10 7 5 -0.0356 0.0126 10 7 6 0.0488 0.0295 10 7 7 -0.1560 0.0202 10 7 8 -0.1974 0.0053 10 7 9 0.1504 -0.0002 10 7 10 0.3995 0.0224 10 7 11 0.2617 0.0485 10 7 12 0.0337 0.0259 10 7 13 -0.0988 -0.0182 10 8 0 -0.3753 -0.0097 10 8 1 -0.2279 -0.0856 10 8 2 -0.0172 -0.0528 10 8 3 0.1689 0.0238 10 8 4 0.1643 0.0259 10 8 5 -0.0668 -0.0273 10 8 6 -0.0919 -0.0554 10 8 7 0.2026 -0.0398 10 8 8 0.2117 -0.0093 10 8 9 -0.2412 -0.0065 10 8 10 -0.5075 -0.0440 10 8 11 -0.3012 -0.0584 10 8 12 -0.0219 -0.0056 10 9 0 0.3101 0.0306 10 9 1 0.2411 0.1074 10 9 2 0.1019 0.0546 10 9 3 -0.0768 -0.0241 10 9 4 -0.0482 -0.0128 10 9 5 0.1926 0.0508 10 9 6 0.1248 0.0775 10 9 7 -0.2689 0.0444 10 9 8 -0.2527 -0.0009 10 9 9 0.2792 0.0073 10 9 10 0.5601 0.0558 10 9 11 0.3204 0.0487 10 10 0 -0.2288 -0.0495 10 10 1 -0.2033 -0.1108 10 10 2 -0.1445 -0.0507 10 10 3 -0.0188 0.0120 10 10 4 -0.0837 -0.0102 10 10 5 -0.2891 -0.0682 10 10 6 -0.1053 -0.0802 10 10 7 0.3500 -0.0287 10 10 8 0.2847 0.0209 10 10 9 -0.2937 -0.0030 10 10 10 -0.5589 -0.0537 10 11 1 0.1440 0.0952 10 11 2 0.1803 0.0484 10 11 3 0.1178 0.0103 10 11 4 0.1824 0.0289 10 11 5 0.3009 0.0650 10 11 6 0.0285 0.0604 10 11 7 -0.4009 0.0023 10 11 8 -0.2644 -0.0405 10 11 9 0.2947 -0.0044 10 12 4 -0.1987 -0.0293 10 12 5 -0.2186 -0.0396 10 12 6 0.0589 -0.0305 11 -3 2 -0.0117 0.0760 11 -3 3 0.0511 0.0976 11 -3 4 0.1561 0.0269 11 -3 5 0.1688 -0.0837 11 -3 6 0.0683 -0.0648 11 -3 7 -0.0692 0.0244 11 -3 8 -0.1959 -0.0009 11 -2 1 -0.0755 -0.0866 11 -2 2 -0.0359 -0.0806 11 -2 3 -0.0601 -0.0518 11 -2 4 -0.1988 0.0243 11 -2 5 -0.2818 0.0765 11 -2 6 -0.1791 0.0369 11 -2 7 0.0633 0.0043 11 -2 8 0.2814 0.0604 11 -2 9 0.2713 0.1063 11 -2 10 0.0334 0.0717 11 -1 0 0.0951 0.0748 11 -1 1 0.2250 0.0819 11 -1 2 0.1076 0.0489 11 -1 3 0.0488 0.0027 11 -1 4 0.2198 -0.0403 11 -1 5 0.3513 -0.0446 11 -1 6 0.2055 -0.0218 11 -1 7 -0.1184 -0.0419 11 -1 8 -0.3397 -0.0902 11 -1 9 -0.2707 -0.0812 11 -1 10 -0.0467 -0.0266 11 -1 11 0.0185 0.0064 11 0 0 -0.2382 -0.0679 11 0 1 -0.4470 -0.0523 11 0 2 -0.1720 -0.0085 11 0 3 0.0094 0.0225 11 0 4 -0.1714 0.0242 11 0 5 -0.3159 0.0104 11 0 6 -0.1334 0.0208 11 0 7 0.1859 0.0650 11 0 8 0.3313 0.0809 11 0 9 0.2348 0.0358 11 0 10 0.1109 -0.0120 11 0 11 0.1410 -0.0305 11 1 0 0.4788 0.0462 11 1 1 0.6766 0.0185 11 1 2 0.1790 -0.0159 11 1 3 -0.1365 -0.0195 11 1 4 0.0369 0.0029 11 1 5 0.1819 0.0100 11 1 6 0.0146 -0.0237 11 1 7 -0.2139 -0.0615 11 1 8 -0.2660 -0.0467 11 1 9 -0.2049 0.0034 11 1 10 -0.2120 0.0292 11 1 11 -0.2800 0.0365 11 1 12 -0.2034 0.0529 11 2 0 -0.7488 -0.0233 11 2 1 -0.8232 0.0018 11 2 2 -0.0968 0.0174 11 2 3 0.3132 0.0025 11 2 4 0.1403 -0.0201 11 2 5 -0.0167 -0.0142 11 2 6 0.0843 0.0198 11 2 7 0.1947 0.0377 11 2 8 0.1952 0.0124 11 2 9 0.2058 -0.0193 11 2 10 0.2959 -0.0238 11 2 11 0.3291 -0.0257 11 2 12 0.1466 -0.0352 11 3 0 0.9422 0.0100 11 3 1 0.8235 -0.0051 11 3 2 -0.0513 -0.0051 11 3 3 -0.4695 0.0110 11 3 4 -0.2793 0.0196 11 3 5 -0.1067 0.0095 11 3 6 -0.1356 -0.0080 11 3 7 -0.1656 -0.0111 11 3 8 -0.1670 0.0043 11 3 9 -0.2223 0.0128 11 3 10 -0.3003 0.0060 11 3 11 -0.2632 0.0077 11 3 12 -0.0511 0.0153 11 4 0 -0.9767 -0.0053 11 4 1 -0.6863 -0.0005 11 4 2 0.1876 -0.0094 11 4 3 0.5217 -0.0142 11 4 4 0.3207 -0.0064 11 4 5 0.1634 -0.0026 11 4 6 0.1585 -0.0049 11 4 7 0.1672 -0.0052 11 4 8 0.1869 -0.0040 11 4 9 0.2138 0.0019 11 4 10 0.1988 0.0101 11 4 11 0.1130 0.0049 11 4 12 -0.0378 -0.0081 11 5 0 0.8468 -0.0002 11 5 1 0.4916 0.0067 11 5 2 -0.2253 0.0227 11 5 3 -0.4324 0.0114 11 5 4 -0.2714 -0.0109 11 5 5 -0.1810 -0.0045 11 5 6 -0.1812 0.0132 11 5 7 -0.2003 0.0116 11 5 8 -0.2207 -0.0001 11 5 9 -0.1537 -0.0101 11 5 10 -0.0205 -0.0153 11 5 11 0.0607 -0.0034 11 5 12 0.0969 0.0186 11 6 0 -0.6260 0.0129 11 6 1 -0.3396 -0.0142 11 6 2 0.1297 -0.0392 11 6 3 0.2426 -0.0089 11 6 4 0.1939 0.0271 11 6 5 0.1964 0.0109 11 6 6 0.1989 -0.0192 11 6 7 0.2261 -0.0190 11 6 8 0.2316 -0.0043 11 6 9 0.0563 0.0071 11 6 10 -0.1704 0.0084 11 6 11 -0.2073 -0.0129 11 6 12 -0.1327 -0.0386 11 7 0 0.4177 -0.0291 11 7 1 0.2858 0.0301 11 7 2 0.0546 0.0619 11 7 3 -0.0469 0.0079 11 7 4 -0.1517 -0.0402 11 7 5 -0.2115 -0.0126 11 7 6 -0.1740 0.0313 11 7 7 -0.2056 0.0359 11 7 8 -0.2163 0.0176 11 7 9 0.0335 0.0014 11 7 10 0.3170 0.0055 11 7 11 0.3076 0.0359 11 8 2 -0.2336 -0.0852 11 8 3 -0.0713 -0.0054 11 8 4 0.1586 0.0468 11 8 5 0.1916 0.0036 11 8 6 0.0771 -0.0538 11 8 7 0.1407 -0.0591 11 8 8 0.2035 -0.0293 11 8 9 -0.0787 -0.0059 11 8 10 -0.3992 -0.0192 11 8 11 -0.3651 -0.0537 11 9 1 0.3466 0.0893 11 9 2 0.3283 0.0983 11 9 3 0.0918 0.0003 11 9 4 -0.1763 -0.0424 11 9 5 -0.1064 0.0176 11 9 6 0.0726 0.0800 11 9 7 -0.0745 0.0753 11 9 8 -0.2194 0.0281 11 9 9 0.0795 0.0013 11 9 10 0.4288 0.0268 11 10 2 -0.3226 -0.0942 11 10 3 -0.0577 0.0033 11 10 4 0.1589 0.0255 11 10 5 -0.0274 -0.0422 11 10 6 -0.2094 -0.0954 11 10 7 0.0510 -0.0733 11 10 8 0.2547 -0.0119 12 -1 5 0.3630 -0.0344 12 -1 6 0.4571 -0.0139 12 0 3 0.1622 0.0024 12 0 4 -0.0558 0.0234 12 0 5 -0.3995 0.0053 12 0 6 -0.4488 -0.0087 12 0 7 -0.1964 0.0307 12 0 8 0.1409 0.0827 12 1 2 0.1480 0.0055 12 1 3 -0.1702 -0.0212 12 1 4 0.0123 -0.0105 12 1 5 0.3236 0.0220 12 1 6 0.3278 0.0150 12 1 7 0.0802 -0.0394 12 1 8 -0.1888 -0.0672 12 1 9 -0.3143 -0.0302 12 2 1 -0.6690 -0.0090 12 2 2 -0.2016 0.0096 12 2 3 0.2223 0.0167 12 2 4 0.0891 -0.0081 12 2 5 -0.1781 -0.0319 12 2 6 -0.1658 -0.0103 12 2 7 0.0269 0.0334 12 2 8 0.2083 0.0358 12 2 9 0.2919 -0.0011 12 2 10 0.2575 -0.0207 12 3 1 0.7531 0.0007 12 3 2 0.1731 -0.0068 12 3 3 -0.3026 -0.0022 12 3 4 -0.1885 0.0162 12 3 5 0.0450 0.0233 12 3 6 0.0299 0.0037 12 3 7 -0.1108 -0.0168 12 3 8 -0.2307 -0.0077 12 3 9 -0.2796 0.0118 12 3 10 -0.2353 0.0101 12 4 1 -0.7059 -0.0013 12 4 2 -0.0803 -0.0038 12 4 3 0.3465 -0.0097 12 4 4 0.2113 -0.0102 12 4 5 0.0196 -0.0049 12 4 6 0.0620 0.0001 12 4 7 0.1892 -0.0001 12 4 8 0.2754 -0.0063 12 4 9 0.2673 -0.0071 12 4 10 0.1600 0.0043 12 5 1 0.5487 0.0014 12 5 2 -0.0061 0.0145 12 5 3 -0.2882 0.0168 12 5 4 -0.1303 -0.0033 12 5 5 -0.0247 -0.0141 12 5 6 -0.1328 -0.0013 12 5 7 -0.2714 0.0111 12 5 8 -0.3244 0.0100 12 5 9 -0.2288 0.0007 12 5 10 -0.0334 -0.0109 12 6 2 0.0130 -0.0267 12 6 3 0.1179 -0.0238 12 6 4 -0.0069 0.0166 12 6 5 0.0253 0.0288 12 6 6 0.2006 0.0004 12 6 7 0.3309 -0.0192 12 6 8 0.3371 -0.0143 12 6 9 0.1533 -0.0028 12 6 10 -0.1090 0.0065 12 7 2 0.0793 0.0459 12 7 3 0.1000 0.0334 12 7 4 0.1113 -0.0267 12 7 5 -0.0645 -0.0367 12 7 6 -0.2455 0.0060 12 7 7 -0.3211 0.0322 12 7 8 -0.2893 0.0265 12 7 9 -0.0629 0.0129 12 8 4 -0.1201 0.0340 12 8 5 0.1321 0.0353 12 8 6 0.2230 -0.0219 12 8 7 0.2200 -0.0526 12 8 8 0.2000 -0.0427 0 0 0 0.0 0.0 ; _shelx_fab_checksum 72140 _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 Mo4 Mo 0.23234(3) 0.97962(2) 0.32208(2) 0.01021(5) Uani 1 1 d . . . . . Mo2 Mo 0.49192(3) 0.91070(2) -0.10334(2) 0.01078(5) Uani 1 1 d . . . . . Mo3 Mo 0.55279(3) 0.77189(2) 0.20041(2) 0.01331(6) Uani 1 1 d . . . . . Mo1 Mo 0.81424(3) 0.83750(2) -0.04428(2) 0.01243(5) Uani 1 1 d . . . . . Ni1 Ni 0.19518(4) 0.97958(3) 0.62521(3) 0.01310(8) Uani 1 1 d . . . . . O4 O 0.7357(2) 0.92183(17) -0.16466(15) 0.0139(4) Uani 1 1 d . . . . . O6 O 0.5539(2) 0.87836(17) 0.03217(15) 0.0134(4) Uani 1 1 d . . . . . O10 O 0.3225(2) 0.83001(17) 0.24322(16) 0.0137(4) Uani 1 1 d . . . . . O13 O 0.2601(2) 0.93347(17) 0.45431(16) 0.0153(4) Uani 1 1 d . . . . . O8 O 0.7583(2) 0.80148(18) 0.12389(16) 0.0155(4) Uani 1 1 d . . . . . O17 O 0.1989(2) 0.16222(17) 0.37578(17) 0.0181(4) Uani 1 1 d . . . . . O2 O 0.2899(2) 0.95618(18) -0.03434(16) 0.0168(4) Uani 1 1 d . . . . . O16 O 0.1868(3) 0.16411(18) 0.56392(17) 0.0217(4) Uani 1 1 d . . . . . O12 O 0.0373(2) 0.99163(17) 0.35316(17) 0.0168(4) Uani 1 1 d . . . . . O1AA O 0.9891(2) 0.8716(2) -0.07114(18) 0.0214(4) Uani 1 1 d . . . . . O14 O 0.4254(3) 0.9463(2) 0.60436(18) 0.0260(5) Uani 1 1 d . . . . . H14A H 0.509477 0.908894 0.539845 0.039 Uiso 1 1 d R U . . . H14B H 0.435446 0.988103 0.655506 0.039 Uiso 1 1 d R U . . . O15 O 0.1200(2) 1.04833(19) 0.79019(17) 0.0210(4) Uani 1 1 d . . . . . H15A H 0.193048 1.072114 0.800589 0.032 Uiso 1 1 d R U . . . H15B H 0.102768 0.989841 0.842447 0.032 Uiso 1 1 d R U . . . O0AA O 0.5246(2) 0.76686(18) -0.15488(18) 0.0206(4) Uani 1 1 d . . . . . O11 O 0.5563(3) 0.7369(2) 0.33875(18) 0.0252(5) Uani 1 1 d . . . . . O5 O 0.8627(3) 0.69007(19) -0.09268(19) 0.0259(5) Uani 1 1 d . . . . . O9 O 0.5725(3) 0.63356(19) 0.14426(19) 0.0259(5) Uani 1 1 d . . . . . N2 N 0.2099(3) 0.5813(2) 0.2038(2) 0.0190(5) Uani 1 1 d . . . . . N4 N 0.2131(3) 0.7902(2) 0.6622(2) 0.0185(5) Uani 1 1 d . . . . . N3 N 0.2306(3) 0.6124(2) 0.5888(2) 0.0185(5) Uani 1 1 d . . . . . C7 C 0.1959(3) 0.2127(2) 0.4659(2) 0.0137(5) Uani 1 1 d . . . . . N1 N 0.1630(4) 0.7168(3) 0.0734(3) 0.0347(7) Uani 1 1 d . . . . . C4 C 0.2086(3) 0.5246(3) 0.3156(2) 0.0170(5) Uani 1 1 d . . . . . C6 C 0.2017(3) 0.3473(2) 0.4449(2) 0.0150(5) Uani 1 1 d . . . . . C5 C 0.1982(3) 0.4026(2) 0.3375(2) 0.0168(5) Uani 1 1 d . . . . . H5 H 0.188957 0.358042 0.281572 0.020 Uiso 1 1 calc R U . . . C2 C 0.1339(4) 0.6983(3) 0.1877(3) 0.0266(7) Uani 1 1 d . . . . . H2 H 0.071577 0.756226 0.246692 0.032 Uiso 1 1 calc R U . . . C9 C 0.2223(3) 0.5929(3) 0.3977(2) 0.0185(6) Uani 1 1 d . . . . . H9 H 0.233155 0.673883 0.380619 0.022 Uiso 1 1 calc R U . . . C8 C 0.2117(3) 0.4145(2) 0.5310(2) 0.0167(5) Uani 1 1 d . . . . . H8 H 0.213077 0.377614 0.602853 0.020 Uiso 1 1 calc R U . . . C13 C 0.3205(4) 0.6970(3) 0.6927(3) 0.0268(7) Uani 1 1 d . . . . . H13 H 0.376318 0.708019 0.737411 0.032 Uiso 1 1 calc R U . . . C11 C 0.1616(4) 0.7357(3) 0.6011(3) 0.0203(6) Uani 1 1 d . . . . . H11 H 0.086067 0.777056 0.569587 0.024 Uiso 1 1 calc R U . . . C10 C 0.2194(3) 0.5375(2) 0.5063(2) 0.0169(5) Uani 1 1 d . . . . . C3 C 0.2887(4) 0.5244(3) 0.0955(3) 0.0278(7) Uani 1 1 d . . . . . H3 H 0.350161 0.443114 0.081452 0.033 Uiso 1 1 calc R U . . . C1 C 0.2596(5) 0.6088(4) 0.0145(3) 0.0363(8) Uani 1 1 d . . . . . H1 H 0.297447 0.596798 -0.066596 0.044 Uiso 1 1 calc R U . . . C12 C 0.3336(4) 0.5861(3) 0.6482(3) 0.0276(7) Uani 1 1 d . . . . . H12 H 0.398365 0.509043 0.656082 0.033 Uiso 1 1 calc R U . . . O7 O 0.4808(2) 0.98387(17) 0.24060(15) 0.0131(4) Uani 1 1 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 Mo4 0.01277(11) 0.01029(10) 0.00736(10) -0.00019(7) -0.00256(8) -0.00401(8) Mo2 0.01396(11) 0.01074(10) 0.00857(10) 0.00079(8) -0.00436(8) -0.00444(8) Mo3 0.01557(12) 0.01100(10) 0.01163(11) 0.00207(8) -0.00385(9) -0.00290(9) Mo1 0.01322(11) 0.01351(11) 0.00992(10) 0.00141(8) -0.00432(8) -0.00270(9) Ni1 0.01760(18) 0.01223(16) 0.01078(16) -0.00085(12) -0.00522(13) -0.00534(13) O4 0.0170(10) 0.0157(9) 0.0085(8) 0.0018(7) -0.0037(7) -0.0050(8) O6 0.0148(9) 0.0165(9) 0.0086(8) 0.0033(7) -0.0045(7) -0.0045(7) O10 0.0162(10) 0.0117(8) 0.0142(9) -0.0010(7) -0.0051(7) -0.0050(7) O13 0.0215(10) 0.0127(9) 0.0107(8) -0.0007(7) -0.0052(8) -0.0030(8) O8 0.0156(10) 0.0181(9) 0.0142(9) 0.0035(7) -0.0073(8) -0.0048(8) O17 0.0310(12) 0.0115(9) 0.0141(9) 0.0000(7) -0.0095(8) -0.0067(8) O2 0.0170(10) 0.0182(9) 0.0151(9) 0.0006(8) -0.0049(8) -0.0059(8) O16 0.0399(13) 0.0145(9) 0.0130(9) 0.0009(7) -0.0093(9) -0.0108(9) O12 0.0145(10) 0.0161(9) 0.0190(10) -0.0009(8) -0.0050(8) -0.0038(8) O1AA 0.0173(10) 0.0261(11) 0.0201(10) 0.0045(8) -0.0062(8) -0.0070(9) O14 0.0254(12) 0.0375(13) 0.0187(10) -0.0043(9) -0.0086(9) -0.0112(10) O15 0.0313(12) 0.0224(10) 0.0135(9) 0.0018(8) -0.0090(9) -0.0126(9) O0AA 0.0255(11) 0.0157(9) 0.0215(10) -0.0028(8) -0.0082(9) -0.0059(8) O11 0.0257(12) 0.0285(11) 0.0183(10) 0.0064(9) -0.0089(9) -0.0032(9) O5 0.0329(13) 0.0174(10) 0.0258(11) -0.0027(9) -0.0106(10) -0.0025(9) O9 0.0280(12) 0.0169(10) 0.0288(12) -0.0049(9) -0.0053(10) -0.0045(9) N2 0.0268(14) 0.0144(11) 0.0161(11) 0.0040(9) -0.0080(10) -0.0069(10) N4 0.0266(13) 0.0170(11) 0.0148(11) 0.0000(9) -0.0078(10) -0.0097(10) N3 0.0273(13) 0.0107(10) 0.0199(12) -0.0013(9) -0.0095(10) -0.0065(10) C7 0.0161(13) 0.0107(11) 0.0134(12) -0.0017(9) -0.0032(10) -0.0040(10) N1 0.0493(19) 0.0307(15) 0.0291(15) 0.0125(12) -0.0223(14) -0.0114(14) C4 0.0224(15) 0.0147(12) 0.0137(12) 0.0021(10) -0.0065(11) -0.0053(11) C6 0.0178(13) 0.0108(12) 0.0141(12) -0.0003(9) -0.0028(10) -0.0041(10) C5 0.0217(14) 0.0138(12) 0.0164(13) 0.0004(10) -0.0074(11) -0.0064(11) C2 0.0366(19) 0.0193(14) 0.0277(16) 0.0065(12) -0.0175(14) -0.0072(13) C9 0.0264(15) 0.0111(12) 0.0199(14) 0.0020(10) -0.0100(12) -0.0060(11) C8 0.0226(15) 0.0135(12) 0.0146(12) 0.0006(10) -0.0072(11) -0.0049(11) C13 0.042(2) 0.0217(15) 0.0253(15) 0.0019(12) -0.0214(15) -0.0087(14) C11 0.0248(15) 0.0139(13) 0.0241(15) -0.0020(11) -0.0100(12) -0.0052(11) C10 0.0214(14) 0.0122(12) 0.0186(13) -0.0031(10) -0.0075(11) -0.0049(11) C3 0.0384(19) 0.0236(15) 0.0169(14) -0.0009(12) -0.0058(14) -0.0064(14) C1 0.049(2) 0.042(2) 0.0180(15) 0.0046(14) -0.0108(15) -0.0153(18) C12 0.042(2) 0.0165(14) 0.0319(17) 0.0041(12) -0.0243(15) -0.0057(14) O7 0.0146(9) 0.0156(9) 0.0100(8) 0.0022(7) -0.0050(7) -0.0052(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' 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' Ni Ni 0.3393 1.1124 '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 O4 Mo4 O17 78.05(7) 2_675 1_565 ? O4 Mo4 O7 71.34(7) 2_675 . ? O10 Mo4 O4 91.33(8) . 2_675 ? O10 Mo4 O17 161.32(8) . 1_565 ? O10 Mo4 O7 77.92(8) . . ? O13 Mo4 O4 155.19(8) . 2_675 ? O13 Mo4 O10 99.58(8) . . ? O13 Mo4 O17 85.02(8) . 1_565 ? O13 Mo4 O7 89.14(8) . . ? O17 Mo4 O7 84.09(7) 1_565 . ? O12 Mo4 O4 94.96(8) . 2_675 ? O12 Mo4 O10 100.92(9) . . ? O12 Mo4 O13 104.62(9) . . ? O12 Mo4 O17 95.32(9) . 1_565 ? O12 Mo4 O7 166.14(8) . . ? O4 Mo2 O6 81.52(6) . 2_675 ? O6 Mo2 O4 73.44(7) . . ? O6 Mo2 O6 76.92(8) . 2_675 ? O2 Mo2 O4 158.40(8) . . ? O2 Mo2 O6 76.91(8) . 2_675 ? O2 Mo2 O6 100.31(8) . . ? O2 Mo2 O7 100.42(8) . 2_675 ? O0AA Mo2 O4 98.06(9) . . ? O0AA Mo2 O6 103.94(9) . . ? O0AA Mo2 O6 178.91(8) . 2_675 ? O0AA Mo2 O2 103.53(10) . . ? O0AA Mo2 O7 104.37(9) . 2_675 ? O7 Mo2 O4 74.54(7) 2_675 . ? O7 Mo2 O6 139.59(8) 2_675 . ? O7 Mo2 O6 74.56(7) 2_675 2_675 ? O6 Mo3 O7 71.91(6) . . ? O10 Mo3 O6 82.81(7) . . ? O10 Mo3 O7 72.55(7) . . ? O8 Mo3 O6 73.08(7) . . ? O8 Mo3 O10 149.97(8) . . ? O8 Mo3 O7 82.95(7) . . ? O11 Mo3 O6 161.22(9) . . ? O11 Mo3 O10 98.12(9) . . ? O11 Mo3 O8 99.17(9) . . ? O11 Mo3 O7 90.38(9) . . ? O9 Mo3 O6 93.78(9) . . ? O9 Mo3 O10 95.96(9) . . ? O9 Mo3 O8 103.11(9) . . ? O9 Mo3 O11 104.74(11) . . ? O9 Mo3 O7 162.36(9) . . ? O4 Mo1 O6 72.39(7) . . ? O4 Mo1 O8 144.30(8) . . ? O4 Mo1 O2 80.40(7) . 2_675 ? O6 Mo1 O2 70.61(7) . 2_675 ? O8 Mo1 O6 73.35(7) . . ? O8 Mo1 O2 79.09(7) . 2_675 ? O1AA Mo1 O4 107.12(9) . . ? O1AA Mo1 O6 153.07(9) . . ? O1AA Mo1 O8 98.88(9) . . ? O1AA Mo1 O2 82.68(8) . 2_675 ? O5 Mo1 O4 97.91(9) . . ? O5 Mo1 O6 101.67(9) . . ? O5 Mo1 O8 98.52(9) . . ? O5 Mo1 O2 172.26(9) . 2_675 ? O5 Mo1 O1AA 105.00(11) . . ? O13 Ni1 O16 86.38(7) . 1_565 ? O13 Ni1 O12 90.40(8) . 2_576 ? O13 Ni1 O14 89.36(8) . . ? O13 Ni1 O15 172.72(8) . . ? O13 Ni1 N4 85.89(8) . . ? O12 Ni1 O16 89.67(8) 2_576 1_565 ? O12 Ni1 N4 90.53(9) 2_576 . ? O14 Ni1 O16 91.77(9) . 1_565 ? O14 Ni1 O12 178.52(9) . 2_576 ? O14 Ni1 N4 88.00(10) . . ? O15 Ni1 O16 86.71(8) . 1_565 ? O15 Ni1 O12 87.25(8) . 2_576 ? O15 Ni1 O14 93.17(9) . . ? O15 Ni1 N4 101.01(9) . . ? N4 Ni1 O16 172.27(8) . 1_565 ? Mo4 O4 Mo2 104.41(8) 2_675 . ? Mo1 O4 Mo4 150.36(10) . 2_675 ? Mo1 O4 Mo2 105.22(8) . . ? Mo2 O6 Mo2 103.08(8) . 2_675 ? Mo2 O6 Mo3 150.56(10) . . ? Mo2 O6 Mo1 104.12(8) . . ? Mo3 O6 Mo2 98.13(7) . 2_675 ? Mo1 O6 Mo2 96.72(7) . 2_675 ? Mo1 O6 Mo3 93.29(7) . . ? Mo4 O10 Mo3 114.58(9) . . ? Mo4 O13 Ni1 144.90(11) . . ? Mo3 O8 Mo1 114.49(9) . . ? C7 O17 Mo4 136.68(17) . 1_545 ? Mo2 O2 Mo1 115.69(9) . 2_675 ? C7 O16 Ni1 131.73(17) . 1_545 ? Mo4 O12 Ni1 173.51(12) . 2_576 ? Ni1 O14 H14A 125.9 . . ? Ni1 O14 H14B 110.2 . . ? H14A O14 H14B 122.3 . . ? Ni1 O15 H15A 110.4 . . ? Ni1 O15 H15B 110.3 . . ? H15A O15 H15B 103.6 . . ? C2 N2 C4 125.5(3) . . ? C2 N2 C3 108.8(3) . . ? C3 N2 C4 125.7(2) . . ? C13 N4 Ni1 133.1(2) . . ? C11 N4 Ni1 114.61(19) . . ? C11 N4 C13 105.3(2) . . ? C11 N3 C10 122.8(2) . . ? C11 N3 C12 106.7(2) . . ? C12 N3 C10 128.9(2) . . ? O17 C7 C6 113.0(2) . . ? O16 C7 O17 127.5(2) . . ? O16 C7 C6 119.5(2) . . ? C2 N1 C1 108.8(3) . . ? C5 C4 N2 119.4(2) . . ? C5 C4 C9 121.6(3) . . ? C9 C4 N2 119.0(2) . . ? C5 C6 C7 118.3(2) . . ? C5 C6 C8 121.0(2) . . ? C8 C6 C7 120.7(2) . . ? C4 C5 C6 118.9(3) . . ? C4 C5 H5 120.6 . . ? C6 C5 H5 120.6 . . ? N2 C2 H2 125.9 . . ? N1 C2 N2 108.1(3) . . ? N1 C2 H2 125.9 . . ? C4 C9 H9 120.7 . . ? C4 C9 C10 118.6(2) . . ? C10 C9 H9 120.7 . . ? C6 C8 H8 120.8 . . ? C10 C8 C6 118.4(3) . . ? C10 C8 H8 120.8 . . ? N4 C13 H13 124.8 . . ? C12 C13 N4 110.4(3) . . ? C12 C13 H13 124.8 . . ? N4 C11 N3 112.3(3) . . ? N4 C11 H11 123.9 . . ? N3 C11 H11 123.9 . . ? C9 C10 N3 116.6(2) . . ? C8 C10 N3 122.0(2) . . ? C8 C10 C9 121.4(3) . . ? N2 C3 H3 126.6 . . ? C1 C3 N2 106.9(3) . . ? C1 C3 H3 126.6 . . ? N1 C1 H1 126.3 . . ? C3 C1 N1 107.5(3) . . ? C3 C1 H1 126.3 . . ? N3 C12 H12 127.3 . . ? C13 C12 N3 105.4(3) . . ? C13 C12 H12 127.3 . . ? Mo4 O7 Mo3 90.54(7) . . ? Mo2 O7 Mo4 109.19(8) 2_675 . ? Mo2 O7 Mo3 114.21(8) 2_675 . ? 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 Mo4 O4 2.0671(17) 2_675 ? Mo4 O10 1.8457(18) . ? Mo4 O13 1.7317(18) . ? Mo4 O17 2.1132(19) 1_565 ? Mo4 O12 1.7250(19) . ? Mo4 O7 2.2164(19) . ? Mo2 O4 2.1984(19) . ? Mo2 O6 2.4682(19) 2_675 ? Mo2 O6 1.9224(18) . ? Mo2 O2 1.7420(19) . ? Mo2 O0AA 1.695(2) . ? Mo2 O7 1.9143(18) 2_675 ? Mo3 O6 2.2533(17) . ? Mo3 O10 1.9916(19) . ? Mo3 O8 1.9375(19) . ? Mo3 O11 1.701(2) . ? Mo3 O9 1.693(2) . ? Mo3 O7 2.3284(19) . ? Mo1 O4 1.9318(18) . ? Mo1 O6 2.2363(19) . ? Mo1 O8 1.9442(18) . ? Mo1 O2 2.3947(19) 2_675 ? Mo1 O1AA 1.718(2) . ? Mo1 O5 1.692(2) . ? Ni1 O13 2.0256(18) . ? Ni1 O16 2.1015(19) 1_565 ? Ni1 O12 2.0716(19) 2_576 ? Ni1 O14 2.047(2) . ? Ni1 O15 2.0311(19) . ? Ni1 N4 2.085(2) . ? O17 C7 1.278(3) . ? O16 C7 1.241(3) . ? O14 H14A 0.9262 . ? O14 H14B 0.8664 . ? O15 H15A 0.8645 . ? O15 H15B 0.8650 . ? N2 C4 1.436(3) . ? N2 C2 1.341(4) . ? N2 C3 1.378(4) . ? N4 C13 1.372(4) . ? N4 C11 1.306(4) . ? N3 C11 1.350(4) . ? N3 C10 1.428(3) . ? N3 C12 1.379(4) . ? C7 C6 1.507(3) . ? N1 C2 1.321(4) . ? N1 C1 1.382(5) . ? C4 C5 1.382(4) . ? C4 C9 1.387(4) . ? C6 C5 1.393(4) . ? C6 C8 1.402(4) . ? C5 H5 0.9300 . ? C2 H2 0.9300 . ? C9 H9 0.9300 . ? C9 C10 1.393(4) . ? C8 H8 0.9300 . ? C8 C10 1.388(4) . ? C13 H13 0.9300 . ? C13 C12 1.362(4) . ? C11 H11 0.9300 . ? C3 H3 0.9300 . ? C3 C1 1.340(5) . ? C1 H1 0.9300 . ? C12 H12 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 Mo4 O17 C7 O16 -13.9(5) 1_545 . . . ? Mo4 O17 C7 C6 167.27(19) 1_545 . . . ? Ni1 O16 C7 O17 7.2(5) 1_545 . . . ? Ni1 O16 C7 C6 -174.01(18) 1_545 . . . ? Ni1 N4 C13 C12 -147.3(2) . . . . ? Ni1 N4 C11 N3 154.0(2) . . . . ? O4 Mo4 O10 Mo3 89.17(10) 2_675 . . . ? O4 Mo4 O13 Ni1 81.0(3) 2_675 . . . ? O4 Mo2 O2 Mo1 5.2(3) . . . 2_675 ? O6 Mo2 O2 Mo1 2.25(8) 2_675 . . 2_675 ? O6 Mo2 O2 Mo1 76.08(10) . . . 2_675 ? O10 Mo4 O13 Ni1 -164.09(19) . . . . ? O13 Mo4 O10 Mo3 -68.46(11) . . . . ? O17 Mo4 O10 Mo3 34.5(3) 1_565 . . . ? O17 Mo4 O13 Ni1 34.17(19) 1_565 . . . ? O17 C7 C6 C5 4.4(4) . . . . ? O17 C7 C6 C8 -175.0(3) . . . . ? O16 C7 C6 C5 -174.5(3) . . . . ? O16 C7 C6 C8 6.1(4) . . . . ? O12 Mo4 O10 Mo3 -175.51(10) . . . . ? O12 Mo4 O13 Ni1 -60.0(2) . . . . ? O0AA Mo2 O2 Mo1 -176.72(10) . . . 2_675 ? N2 C4 C5 C6 178.1(3) . . . . ? N2 C4 C9 C10 179.4(3) . . . . ? N2 C3 C1 N1 -0.1(4) . . . . ? N4 C13 C12 N3 -0.2(4) . . . . ? C7 C6 C5 C4 -177.9(3) . . . . ? C7 C6 C8 C10 178.9(3) . . . . ? C4 N2 C2 N1 180.0(3) . . . . ? C4 N2 C3 C1 179.9(3) . . . . ? C4 C9 C10 N3 -178.7(3) . . . . ? C4 C9 C10 C8 3.5(4) . . . . ? C6 C8 C10 N3 -179.7(3) . . . . ? C6 C8 C10 C9 -2.0(4) . . . . ? C5 C4 C9 C10 -2.5(4) . . . . ? C5 C6 C8 C10 -0.6(4) . . . . ? C2 N2 C4 C5 138.9(3) . . . . ? C2 N2 C4 C9 -42.9(4) . . . . ? C2 N2 C3 C1 0.3(4) . . . . ? C2 N1 C1 C3 -0.1(4) . . . . ? C9 C4 C5 C6 0.0(4) . . . . ? C8 C6 C5 C4 1.6(4) . . . . ? C13 N4 C11 N3 -0.7(3) . . . . ? C11 N4 C13 C12 0.5(4) . . . . ? C11 N3 C10 C9 37.5(4) . . . . ? C11 N3 C10 C8 -144.7(3) . . . . ? C11 N3 C12 C13 -0.2(4) . . . . ? C10 N3 C11 N4 -166.5(3) . . . . ? C10 N3 C12 C13 165.8(3) . . . . ? C3 N2 C4 C5 -40.6(4) . . . . ? C3 N2 C4 C9 137.5(3) . . . . ? C3 N2 C2 N1 -0.4(4) . . . . ? C1 N1 C2 N2 0.3(4) . . . . ? C12 N3 C11 N4 0.6(4) . . . . ? C12 N3 C10 C9 -126.5(3) . . . . ? C12 N3 C10 C8 51.3(4) . . . . ? O7 Mo4 O10 Mo3 18.58(8) . . . . ? O7 Mo4 O13 Ni1 118.3(2) . . . . ? O7 Mo2 O2 Mo1 -69.04(10) 2_675 . . 2_675 ? 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 41.0 6.5 ?