#------------------------------------------------------------------------------ #$Date: 2021-11-06 22:31:12 +0200 (Sat, 06 Nov 2021) $ #$Revision: 270480 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/06/10/7061009.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_7061009 loop_ _publ_author_name 'Kuzman, Dino' 'Damjanovi\'c, Vladimir' 'Stilinovi\'c, Vladimir' 'Cindri\'c, Marina' 'Vrdoljak, Vi\ 2\s(I)' _cod_data_source_file d1nj03280a2.cif _cod_data_source_block 9 _cod_depositor_comments 'Adding full bibliography for 7061007--7061013.cif.' _cod_original_cell_volume 6441.4(3) _cod_original_sg_symbol_H-M 'I 41/a' _cod_database_code 7061009 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'Mo12 Si O50 Co4 C20' _chemical_oxdiff_usercomment MoSi_HCl _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.629 _shelx_estimated_absorpt_t_min 0.549 _reflns_odcompleteness_completeness 99.64 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 30.44 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All H(H,H) groups, All N(H,H,H) groups At 1.5 times of: All O(H) groups, All O(H,H) groups 2. Restrained distances O5-H2W 2.336 with sigma of 0.05 3.a Free rotating group: O1W(H1WA,H1WB), O2W(H2W) 3.b Idealised Me refined as rotating group: N3(H3A,H3B,H3C), N2(H2A,H2B,H2C), N1(H1A,H1B,H1C), N4(H4A,H4B,H4C) ; _shelx_res_file ; TITL exp_4770_a.res in I4(1)/a exp_4770.res created by SHELXL-2018/3 at 19:00:59 on 08-May-2021 REM Old TITL exp_4770 in I4(1)/a REM SHELXT solution in I4(1)/a: R1 0.142, Rweak 0.007, Alpha 0.027 REM 1.312 for 86 systematic absences, Orientation as input REM Formula found by SHELXT: C36 O50 Si Co16 CELL 0.71073 16.6637 16.6637 23.1974 90 90 90 ZERR 4 0.0003 0.0003 0.0006 0 0 0 LATT 2 SYMM 0.5-X,-Y,0.5+Z SYMM 0.75-Y,0.25+X,0.25+Z SYMM 0.75+Y,0.75-X,0.75+Z SFAC C H Co Mo N O Si UNIT 32 240 16 48 64 248 4 DFIX 2.336 0.05 O5 H2W L.S. 4 PLAN 5 SIZE 0.2 0.15 0.17 TEMP 24.85 CONF list 4 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.029000 20.433001 EXTI 0.000052 FVAR 0.07261 MO3 4 0.396912 0.858001 0.731781 11.00000 0.02548 0.02696 = 0.02591 -0.00817 0.01013 -0.00385 MO1 4 0.402353 0.636675 0.732211 11.00000 0.02553 0.02718 = 0.03674 0.01251 0.01391 0.00376 MO2 4 0.288049 0.745034 0.619070 11.00000 0.01556 0.04371 = 0.02560 -0.00445 0.00288 -0.00184 CO1 3 0.150083 0.459198 0.603555 11.00000 0.02087 0.01977 = 0.01983 0.00111 -0.00222 -0.00052 SI1 7 0.500000 0.750000 0.625000 10.25000 0.01246 0.01246 = 0.01312 0.00000 0.00000 0.00000 O4 6 0.329474 0.666588 0.673095 11.00000 0.01988 0.02093 = 0.02385 0.00120 -0.00045 -0.00078 O1 6 0.502339 0.670122 0.665652 11.00000 0.01753 0.01541 = 0.01745 0.00162 -0.00024 0.00045 O10 6 0.495385 0.880169 0.772094 11.00000 0.02355 0.02555 = 0.02008 -0.00430 -0.00123 0.00045 O9 6 0.412492 0.956997 0.689744 11.00000 0.02140 0.01945 = 0.02401 -0.00087 0.00190 0.00276 O3 6 0.406890 0.747300 0.752162 11.00000 0.02390 0.02058 = 0.02236 0.00036 0.00179 0.00061 O7 6 0.325310 0.822768 0.672452 11.00000 0.02155 0.02051 = 0.02246 -0.00236 -0.00102 0.00099 O6 6 0.288250 0.824179 0.558942 11.00000 0.01927 0.02374 = 0.02645 0.00113 -0.00220 0.00292 O11 6 0.165534 0.472376 0.522340 11.00000 0.02501 0.02627 = 0.02346 0.00341 0.00003 -0.00329 O12 6 0.047492 0.416861 0.584095 11.00000 0.02083 0.03512 = 0.02182 -0.00153 0.00021 -0.00238 O8 6 0.330475 0.892146 0.780994 11.00000 0.02571 0.03132 = 0.02698 -0.00697 0.00704 -0.00121 O2 6 0.340707 0.600038 0.783379 11.00000 0.03036 0.03205 = 0.03797 0.01166 0.01236 0.00139 O5 6 0.188900 0.741064 0.632937 11.00000 0.01744 0.04602 = 0.03148 -0.00167 0.00170 -0.00203 O14 6 -0.028600 0.395174 0.507151 11.00000 0.02415 0.04631 = 0.03414 -0.00218 -0.00719 -0.00342 N3 5 0.195818 0.352015 0.594950 11.00000 0.02797 0.02218 = 0.02887 0.00080 -0.00186 0.00137 AFIX 137 H3A 2 0.167046 0.324236 0.569521 11.00000 0.06357 H3B 2 0.195041 0.326954 0.628826 11.00000 -1.20000 H3C 2 0.246219 0.355987 0.582579 11.00000 -1.20000 AFIX 0 O13 6 0.103435 0.441434 0.440104 11.00000 0.04624 0.04346 = 0.02090 0.00283 -0.00160 -0.00667 N2 5 0.101303 0.566672 0.606254 11.00000 0.04184 0.02702 = 0.02940 -0.00336 -0.01114 0.00695 AFIX 137 H2A 2 0.069889 0.573466 0.575611 11.00000 -1.20000 H2B 2 0.139787 0.603705 0.606144 11.00000 -1.20000 H2C 2 0.072169 0.571453 0.638225 11.00000 -1.20000 AFIX 0 N1 5 0.129424 0.440447 0.685039 11.00000 0.03000 0.02831 = 0.02336 0.00001 -0.00101 -0.00016 AFIX 137 H1A 2 0.134695 0.388385 0.692716 11.00000 -1.20000 H1B 2 0.079768 0.456122 0.693573 11.00000 -1.20000 H1C 2 0.164362 0.468263 0.706082 11.00000 -1.20000 AFIX 0 N4 5 0.256132 0.501024 0.621454 11.00000 0.02674 0.02593 = 0.03074 0.00112 -0.00303 -0.00519 AFIX 137 H4A 2 0.283248 0.508945 0.588894 11.00000 -1.20000 H4B 2 0.282378 0.465946 0.643398 11.00000 -1.20000 H4C 2 0.251308 0.547324 0.640263 11.00000 -1.20000 AFIX 6 O1W 6 0.120709 0.261442 0.495579 11.00000 0.07941 0.04372 = 0.04944 -0.00236 -0.00002 0.00346 H1WA 2 0.076057 0.239950 0.486989 11.00000 -1.50000 H1WB 2 0.139328 0.285719 0.466234 11.00000 -1.50000 AFIX 0 C2 1 0.034679 0.415342 0.529779 11.00000 0.02254 0.02306 = 0.02502 0.00217 -0.00158 0.00139 C1 1 0.106321 0.444951 0.492869 11.00000 0.02894 0.02151 = 0.02157 0.00300 -0.00045 0.00134 AFIX 6 O2W 6 0.000000 0.750000 0.611896 10.50000 0.07942 0.17322 = 0.10280 0.00000 0.00000 0.03144 H2W 2 0.045133 0.750247 0.628995 11.00000 -1.50000 AFIX 0 HKLF 4 REM exp_4770_a.res in I4(1)/a REM wR2 = 0.0746, GooF = S = 1.087, Restrained GooF = 1.087 for all data REM R1 = 0.0315 for 4632 Fo > 4sig(Fo) and 0.0411 for all 5493 data REM 245 parameters refined using 1 restraints END WGHT 0.0289 20.4490 REM Highest difference peak 1.658, deepest hole -1.389, 1-sigma level 0.123 Q1 1 0.0000 0.2500 0.6250 10.25000 0.05 1.66 Q2 1 0.2978 0.5311 0.6253 11.00000 0.05 0.89 Q3 1 0.0000 0.7500 0.6608 10.50000 0.05 0.78 Q4 1 0.3706 0.8840 0.7736 11.00000 0.05 0.56 Q5 1 0.1820 0.3450 0.4847 11.00000 0.05 0.53 ; _shelx_res_checksum 19689 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.148 _oxdiff_exptl_absorpt_empirical_full_min 0.929 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' 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 Mo3 Mo 0.39691(2) 0.85800(2) 0.73178(2) 0.02611(7) Uani 1 1 d . . . . . Mo1 Mo 0.40235(2) 0.63667(2) 0.73221(2) 0.02981(7) Uani 1 1 d . . . . . Mo2 Mo 0.28805(2) 0.74503(2) 0.61907(2) 0.02829(7) Uani 1 1 d . . . . . Co1 Co 0.15008(2) 0.45920(2) 0.60355(2) 0.02016(8) Uani 1 1 d . . . . . Si1 Si 0.500000 0.750000 0.625000 0.0127(2) Uani 1 4 d S T P . . O4 O 0.32947(11) 0.66659(11) 0.67310(8) 0.0216(4) Uani 1 1 d . . . . . O1 O 0.50234(10) 0.67012(10) 0.66565(7) 0.0168(3) Uani 1 1 d . . . . . O10 O 0.49538(12) 0.88017(12) 0.77209(8) 0.0231(4) Uani 1 1 d . . . . . O9 O 0.41249(11) 0.95700(11) 0.68974(8) 0.0216(4) Uani 1 1 d . . . . . O3 O 0.40689(12) 0.74730(11) 0.75216(8) 0.0223(4) Uani 1 1 d . . . . . O7 O 0.32531(11) 0.82277(11) 0.67245(8) 0.0215(4) Uani 1 1 d . . . . . O6 O 0.28825(11) 0.82418(12) 0.55894(8) 0.0232(4) Uani 1 1 d . . . . . O11 O 0.16553(12) 0.47238(12) 0.52234(9) 0.0249(4) Uani 1 1 d . . . . . O12 O 0.04749(12) 0.41686(13) 0.58410(8) 0.0259(4) Uani 1 1 d . . . . . O8 O 0.33047(12) 0.89215(13) 0.78099(9) 0.0280(4) Uani 1 1 d . . . . . O2 O 0.34071(13) 0.60004(14) 0.78338(10) 0.0335(5) Uani 1 1 d . . . . . O5 O 0.18890(12) 0.74106(15) 0.63294(9) 0.0316(5) Uani 1 1 d D . . . . O14 O -0.02860(13) 0.39517(15) 0.50715(10) 0.0349(5) Uani 1 1 d . . . . . N3 N 0.19582(15) 0.35201(14) 0.59495(11) 0.0263(5) Uani 1 1 d . . . . . H3A H 0.167046 0.324236 0.569521 0.064(14) Uiso 1 1 calc R . . . . H3B H 0.195041 0.326954 0.628826 0.076 Uiso 1 1 calc R U . . . H3C H 0.246219 0.355987 0.582579 0.076 Uiso 1 1 calc R U . . . O13 O 0.10344(15) 0.44143(15) 0.44010(9) 0.0369(5) Uani 1 1 d . . . . . N2 N 0.10130(17) 0.56667(16) 0.60625(12) 0.0328(6) Uani 1 1 d . . . . . H2A H 0.069889 0.573466 0.575611 0.039 Uiso 1 1 calc R U . . . H2B H 0.139787 0.603705 0.606144 0.039 Uiso 1 1 calc R U . . . H2C H 0.072169 0.571453 0.638225 0.039 Uiso 1 1 calc R U . . . N1 N 0.12942(15) 0.44045(15) 0.68504(10) 0.0272(5) Uani 1 1 d . . . . . H1A H 0.134695 0.388385 0.692716 0.033 Uiso 1 1 calc R U . . . H1B H 0.079768 0.456122 0.693573 0.033 Uiso 1 1 calc R U . . . H1C H 0.164362 0.468263 0.706082 0.033 Uiso 1 1 calc R U . . . N4 N 0.25613(15) 0.50102(15) 0.62145(11) 0.0278(5) Uani 1 1 d . . . . . H4A H 0.283248 0.508945 0.588894 0.033 Uiso 1 1 calc R U . . . H4B H 0.282378 0.465946 0.643398 0.033 Uiso 1 1 calc R U . . . H4C H 0.251308 0.547324 0.640263 0.033 Uiso 1 1 calc R U . . . O1W O 0.1207(2) 0.26144(19) 0.49558(13) 0.0575(8) Uani 1 1 d G . . . . H1WA H 0.076057 0.239950 0.486989 0.086 Uiso 1 1 d G U . . . H1WB H 0.139328 0.285719 0.466234 0.086 Uiso 1 1 d G U . . . C2 C 0.03468(16) 0.41534(17) 0.52978(12) 0.0235(5) Uani 1 1 d . . . . . C1 C 0.10632(18) 0.44495(16) 0.49287(12) 0.0240(5) Uani 1 1 d . . . . . O2W O 0.000000 0.750000 0.6119(4) 0.118(3) Uani 1 2 d GS T P . . H2W H 0.045133 0.750247 0.628995 0.178 Uiso 1 1 d DG U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo3 0.02548(12) 0.02696(12) 0.02591(12) -0.00817(9) 0.01013(9) -0.00385(9) Mo1 0.02553(12) 0.02718(13) 0.03674(14) 0.01251(10) 0.01391(10) 0.00376(9) Mo2 0.01556(11) 0.04371(16) 0.02560(12) -0.00445(10) 0.00288(9) -0.00184(9) Co1 0.02087(17) 0.01977(17) 0.01983(16) 0.00111(13) -0.00222(13) -0.00052(13) Si1 0.0125(3) 0.0125(3) 0.0131(5) 0.000 0.000 0.000 O4 0.0199(8) 0.0209(9) 0.0238(9) 0.0012(7) -0.0004(7) -0.0008(7) O1 0.0175(8) 0.0154(8) 0.0174(8) 0.0016(6) -0.0002(6) 0.0005(6) O10 0.0235(9) 0.0255(9) 0.0201(8) -0.0043(7) -0.0012(7) 0.0004(7) O9 0.0214(9) 0.0194(8) 0.0240(9) -0.0009(7) 0.0019(7) 0.0028(7) O3 0.0239(9) 0.0206(9) 0.0224(9) 0.0004(7) 0.0018(7) 0.0006(7) O7 0.0216(9) 0.0205(9) 0.0225(9) -0.0024(7) -0.0010(7) 0.0010(7) O6 0.0193(9) 0.0237(9) 0.0265(9) 0.0011(7) -0.0022(7) 0.0029(7) O11 0.0250(9) 0.0263(10) 0.0235(9) 0.0034(8) 0.0000(8) -0.0033(7) O12 0.0208(9) 0.0351(11) 0.0218(9) -0.0015(8) 0.0002(7) -0.0024(8) O8 0.0257(10) 0.0313(11) 0.0270(10) -0.0070(8) 0.0070(8) -0.0012(8) O2 0.0304(11) 0.0320(11) 0.0380(12) 0.0117(9) 0.0124(9) 0.0014(9) O5 0.0174(9) 0.0460(13) 0.0315(11) -0.0017(9) 0.0017(8) -0.0020(9) O14 0.0241(10) 0.0463(14) 0.0341(11) -0.0022(10) -0.0072(9) -0.0034(9) N3 0.0280(12) 0.0222(11) 0.0289(12) 0.0008(9) -0.0019(10) 0.0014(9) O13 0.0462(14) 0.0435(13) 0.0209(10) 0.0028(9) -0.0016(9) -0.0067(11) N2 0.0418(15) 0.0270(12) 0.0294(12) -0.0034(10) -0.0111(11) 0.0069(11) N1 0.0300(12) 0.0283(12) 0.0234(11) 0.0000(9) -0.0010(9) -0.0002(10) N4 0.0267(12) 0.0259(12) 0.0307(12) 0.0011(10) -0.0030(10) -0.0052(9) O1W 0.079(2) 0.0437(17) 0.0494(17) -0.0024(13) 0.0000(16) 0.0035(15) C2 0.0225(12) 0.0231(12) 0.0250(12) 0.0022(10) -0.0016(10) 0.0014(10) C1 0.0289(13) 0.0215(12) 0.0216(12) 0.0030(10) -0.0004(10) 0.0013(10) O2W 0.079(5) 0.173(8) 0.103(5) 0.000 0.000 0.031(5) 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' Co Co 0.3494 0.9721 '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' Si Si 0.0817 0.0704 '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 O10 Mo3 O1 75.12(7) . 6_564 ? O10 Mo3 O9 88.10(8) . . ? O9 Mo3 O1 75.05(7) . 6_564 ? O3 Mo3 O1 84.59(7) . 6_564 ? O3 Mo3 O10 89.48(8) . . ? O3 Mo3 O9 159.43(8) . . ? O3 Mo3 O7 86.33(8) . . ? O7 Mo3 O1 85.05(7) . 6_564 ? O7 Mo3 O10 160.04(8) . . ? O7 Mo3 O9 89.01(8) . . ? O8 Mo3 O1 171.30(8) . 6_564 ? O8 Mo3 O10 99.54(9) . . ? O8 Mo3 O9 98.13(9) . . ? O8 Mo3 O3 102.41(9) . . ? O8 Mo3 O7 100.41(9) . . ? O4 Mo1 O1 85.20(7) . . ? O4 Mo1 O10 159.25(8) . 6_564 ? O4 Mo1 O3 86.95(8) . . ? O4 Mo1 O6 89.74(8) . 12_767 ? O10 Mo1 O1 74.11(7) 6_564 . ? O3 Mo1 O1 84.34(7) . . ? O3 Mo1 O10 89.39(8) . 6_564 ? O3 Mo1 O6 158.78(8) . 12_767 ? O6 Mo1 O1 74.50(7) 12_767 . ? O6 Mo1 O10 86.32(8) 12_767 6_564 ? O2 Mo1 O4 102.36(10) . . ? O2 Mo1 O1 170.42(9) . . ? O2 Mo1 O10 98.38(10) . 6_564 ? O2 Mo1 O3 101.77(10) . . ? O2 Mo1 O6 99.41(10) . 12_767 ? O4 Mo2 O1 84.28(7) . 15_566 ? O4 Mo2 O9 87.79(8) . 12_767 ? O9 Mo2 O1 74.42(7) 12_767 15_566 ? O7 Mo2 O4 85.52(8) . . ? O7 Mo2 O1 84.50(7) . 15_566 ? O7 Mo2 O9 158.43(8) . 12_767 ? O7 Mo2 O6 90.26(8) . . ? O6 Mo2 O4 158.86(8) . . ? O6 Mo2 O1 74.68(7) . 15_566 ? O6 Mo2 O9 88.62(8) . 12_767 ? O5 Mo2 O4 101.50(10) . . ? O5 Mo2 O1 170.84(9) . 15_566 ? O5 Mo2 O9 98.53(10) . 12_767 ? O5 Mo2 O7 102.90(10) . . ? O5 Mo2 O6 99.64(10) . . ? O11 Co1 N3 87.24(10) . . ? O11 Co1 N2 89.00(10) . . ? O11 Co1 N1 176.35(10) . . ? O11 Co1 N4 92.68(10) . . ? O12 Co1 O11 85.98(8) . . ? O12 Co1 N3 89.27(10) . . ? O12 Co1 N2 88.50(11) . . ? O12 Co1 N1 90.68(10) . . ? O12 Co1 N4 178.36(10) . . ? N3 Co1 N2 175.75(11) . . ? N1 Co1 N3 91.23(11) . . ? N1 Co1 N2 92.41(11) . . ? N4 Co1 N3 89.71(11) . . ? N4 Co1 N2 92.43(12) . . ? N4 Co1 N1 90.62(11) . . ? O1 Si1 O1 109.51(6) 6_564 12_767 ? O1 Si1 O1 109.51(6) 12_767 . ? O1 Si1 O1 109.39(12) 6_564 . ? O1 Si1 O1 109.51(6) 15_566 . ? O1 Si1 O1 109.51(6) 15_566 6_564 ? O1 Si1 O1 109.39(12) 15_566 12_767 ? Mo1 O4 Mo2 150.70(11) . . ? Mo3 O1 Mo1 91.77(6) 6_564 . ? Mo3 O1 Mo2 91.38(6) 6_564 12_767 ? Mo1 O1 Mo2 90.94(6) . 12_767 ? Si1 O1 Mo3 124.32(9) . 6_564 ? Si1 O1 Mo1 123.98(9) . . ? Si1 O1 Mo2 124.59(9) . 12_767 ? Mo3 O10 Mo1 118.99(9) . 6_564 ? Mo3 O9 Mo2 119.10(9) . 15_566 ? Mo1 O3 Mo3 150.64(11) . . ? Mo2 O7 Mo3 152.03(11) . . ? Mo2 O6 Mo1 119.87(9) . 15_566 ? C1 O11 Co1 112.32(18) . . ? C2 O12 Co1 113.02(18) . . ? Co1 N3 H3A 109.5 . . ? Co1 N3 H3B 109.5 . . ? Co1 N3 H3C 109.5 . . ? H3A N3 H3B 109.5 . . ? H3A N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? Co1 N2 H2A 109.5 . . ? Co1 N2 H2B 109.5 . . ? Co1 N2 H2C 109.5 . . ? H2A N2 H2B 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? Co1 N1 H1A 109.5 . . ? Co1 N1 H1B 109.5 . . ? Co1 N1 H1C 109.5 . . ? H1A N1 H1B 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? Co1 N4 H4A 109.5 . . ? Co1 N4 H4B 109.5 . . ? Co1 N4 H4C 109.5 . . ? H4A N4 H4B 109.5 . . ? H4A N4 H4C 109.5 . . ? H4B N4 H4C 109.5 . . ? H1WA O1W H1WB 109.4 . . ? O12 C2 C1 114.2(2) . . ? O14 C2 O12 124.9(3) . . ? O14 C2 C1 120.9(3) . . ? O11 C1 C2 114.3(2) . . ? O13 C1 O11 125.3(3) . . ? O13 C1 C2 120.4(3) . . ? H2W O2W H2W 124.4 . 6_464 ? 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 Mo3 O1 2.3219(17) 6_564 ? Mo3 O10 1.9245(19) . ? Mo3 O9 1.9338(19) . ? Mo3 O3 1.9116(19) . ? Mo3 O7 1.9137(19) . ? Mo3 O8 1.689(2) . ? Mo1 O4 1.8984(19) . ? Mo1 O1 2.3389(17) . ? Mo1 O10 1.9592(19) 6_564 ? Mo1 O3 1.9021(19) . ? Mo1 O6 1.937(2) 12_767 ? Mo1 O2 1.684(2) . ? Mo2 O4 1.9380(19) . ? Mo2 O1 2.3440(17) 15_566 ? Mo2 O9 1.9391(19) 12_767 ? Mo2 O7 1.8966(19) . ? Mo2 O6 1.920(2) . ? Mo2 O5 1.685(2) . ? Co1 O11 1.914(2) . ? Co1 O12 1.904(2) . ? Co1 N3 1.952(2) . ? Co1 N2 1.968(3) . ? Co1 N1 1.947(2) . ? Co1 N4 1.944(2) . ? Si1 O1 1.6317(17) 12_767 ? Si1 O1 1.6317(17) . ? Si1 O1 1.6317(17) 6_564 ? Si1 O1 1.6317(17) 15_566 ? O11 C1 1.284(3) . ? O12 C2 1.278(3) . ? O14 C2 1.225(3) . ? N3 H3A 0.8900 . ? N3 H3B 0.8900 . ? N3 H3C 0.8900 . ? O13 C1 1.226(3) . ? N2 H2A 0.8900 . ? N2 H2B 0.8900 . ? N2 H2C 0.8900 . ? N1 H1A 0.8900 . ? N1 H1B 0.8900 . ? N1 H1C 0.8900 . ? N4 H4A 0.8900 . ? N4 H4B 0.8900 . ? N4 H4C 0.8900 . ? O1W H1WA 0.8495 . ? O1W H1WB 0.8505 . ? C2 C1 1.550(4) . ? O2W H2W 0.8503 . ? O2W H2W 0.85(7) 6_464 ? 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 Co1 O11 C1 O13 -175.2(2) . . . . ? Co1 O11 C1 C2 5.1(3) . . . . ? Co1 O12 C2 O14 -175.5(2) . . . . ? Co1 O12 C2 C1 2.2(3) . . . . ? O4 Mo2 O7 Mo3 28.4(2) . . . . ? O1 Mo1 O4 Mo2 -57.7(2) . . . . ? O1 Mo2 O7 Mo3 -56.2(2) 15_566 . . . ? O1 Si1 O1 Mo3 179.76(12) 15_566 . . 6_564 ? O1 Si1 O1 Mo3 -60.21(8) 6_564 . . 6_564 ? O1 Si1 O1 Mo3 59.81(4) 12_767 . . 6_564 ? O1 Si1 O1 Mo1 -179.86(12) 12_767 . . . ? O1 Si1 O1 Mo1 -59.90(4) 15_566 . . . ? O1 Si1 O1 Mo1 60.12(8) 6_564 . . . ? O1 Si1 O1 Mo2 179.38(14) 6_564 . . 12_767 ? O1 Si1 O1 Mo2 59.36(14) 15_566 . . 12_767 ? O1 Si1 O1 Mo2 -60.59(14) 12_767 . . 12_767 ? O10 Mo1 O4 Mo2 -53.3(4) 6_564 . . . ? O9 Mo2 O7 Mo3 -43.9(4) 12_767 . . . ? O3 Mo1 O4 Mo2 26.9(2) . . . . ? O6 Mo1 O4 Mo2 -132.1(2) 12_767 . . . ? O6 Mo2 O7 Mo3 -130.8(2) . . . . ? O12 C2 C1 O11 -5.1(4) . . . . ? O12 C2 C1 O13 175.2(3) . . . . ? O2 Mo1 O4 Mo2 128.3(2) . . . . ? O5 Mo2 O7 Mo3 129.2(2) . . . . ? O14 C2 C1 O11 172.7(3) . . . . ? O14 C2 C1 O13 -7.0(4) . . . . ?