#------------------------------------------------------------------------------ #$Date: 2020-02-11 04:10:46 +0200 (Tue, 11 Feb 2020) $ #$Revision: 248017 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/72/1557285.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_1557285 loop_ _publ_author_name 'Du, Jing' 'Lang, Zhong-Ling' 'Ma, Yuanyuan' 'Tan, Huaqiao' 'Liu, Bailing' 'Wang, Yong-Hui' 'Kang, Zhenhui' 'Li, Yang-Guang' _publ_section_title ; Polyoxometalate-Based Electron Transfer Modulation for Efficient Electrocatalytic Carbon Dioxide Reduction ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/C9SC05392A _journal_year 2020 _chemical_formula_moiety 'Mo12 O40 P, 3(C15 H11 Mn N3 O3), 2(C2 H3 N)' _chemical_formula_sum 'C49 H39 Mn3 Mo12 N11 O49 P' _chemical_formula_weight 2912.98 _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 geom _atom_sites_solution_primary direct _audit_creation_date 2019-01-23 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-01-24 deposited with the CCDC. 2020-02-03 downloaded from the CCDC. ; _cell_angle_alpha 79.875(2) _cell_angle_beta 88.908(2) _cell_angle_gamma 87.011(2) _cell_formula_units_Z 2 _cell_length_a 13.0340(6) _cell_length_b 15.6737(6) _cell_length_c 20.2719(9) _cell_measurement_reflns_used 9857 _cell_measurement_temperature 273(2) _cell_measurement_theta_max 27.08 _cell_measurement_theta_min 2.58 _cell_volume 4071.1(3) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _diffrn_ambient_temperature 273.15 _diffrn_measured_fraction_theta_full 0.998 _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 0.0736 _diffrn_reflns_av_unetI/netI 0.0611 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 74286 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.201 _diffrn_reflns_theta_min 2.229 _exptl_absorpt_coefficient_mu 2.351 _exptl_absorpt_correction_type none _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 2.376 _exptl_crystal_description block _exptl_crystal_F_000 2792 _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _refine_diff_density_max 1.137 _refine_diff_density_min -1.314 _refine_diff_density_rms 0.157 _refine_ls_extinction_coef 0.00027(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/1 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1132 _refine_ls_number_reflns 17989 _refine_ls_number_restraints 4334 _refine_ls_restrained_S_all 0.974 _refine_ls_R_factor_all 0.0955 _refine_ls_R_factor_gt 0.0481 _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^)+(0.0231P)^2^+27.1647P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0871 _refine_ls_wR_factor_ref 0.1070 _reflns_Friedel_coverage 0.000 _reflns_number_gt 11784 _reflns_number_total 17989 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc05392a2.cif _cod_data_source_block 1 _cod_database_code 1557285 _shelx_shelxl_version_number 2018/1 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.580 _shelx_estimated_absorpt_t_min 0.529 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances N10-C46 1.14 with sigma of 0.01 C47-C46 1.38 with sigma of 0.01 3. Uiso/Uaniso restraints and constraints C27 \\sim C6 \\sim C5 \\sim C7 \\sim C4 \\sim C11 \\sim C20 \\sim C35 \\sim C10 \\sim C17 \\sim C38 \\sim C40 \\sim C44 \\sim C28 \\sim C3 \\sim C36 \\sim C2 \\sim C29 \\sim C39 \\sim C19 \\sim C32 \\sim C16 \\sim C30 \\sim C45 \\sim C37 \\sim C25 \\sim C18 \\sim C1 \\sim C21 \\sim C43 \\sim C33 \\sim C8 \\sim C9 \\sim C31 \\sim C12 \\sim C34 \\sim C14 \\sim C22 \\sim C23 \\sim C24 \\sim C15 \\sim C26 \\sim C13 \\sim C46 \\sim C47 \\sim C49 \\sim C48 \\sim C41 \\sim C42 \\sim N9 \\sim N2 \\sim N8 \\sim N4 \\sim N1 \\sim N5 \\sim N7 \\sim N6 \\sim N3 \\sim N11 \\sim N10: within 5A with sigma of 0.01 and sigma for terminal atoms of 0.02 O10 \\sim O15 \\sim O26 \\sim O30 \\sim O3 \\sim O33 \\sim O29 \\sim O9 \\sim O21 \\sim O34 \\sim O24 \\sim O38 \\sim O8 \\sim O12 \\sim O19 \\sim O32 \\sim O20 \\sim O40 \\sim O13 \\sim O4 \\sim O5 \\sim O2 \\sim O23 \\sim O27 \\sim O16 \\sim O37 \\sim O22 \\sim O17 \\sim O28 \\sim O11 \\sim O36 \\sim O39 \\sim O31 \\sim O7 \\sim O1 \\sim O14 \\sim O35 \\sim O25 \\sim O45 \\sim O46 \\sim O41 \\sim O18 \\sim O49 \\sim O6 \\sim O42 \\sim O44 \\sim O43 \\sim O47 \\sim O48: within 5A with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(O49) \\sim Ueq, Uanis(N10) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.02 4.a Aromatic/amide H refined with riding coordinates: C7(H7), C4(H4), C10(H10), C17(H17), C38(H38), C40(H40), C3(H3), C2(H2), C39(H39), C19(H19), C32(H32), C16(H16), C37(H37), C25(H25), C18(H18), C1(H1), C33(H33), C8(H8), C9(H9), C31(H31), C34(H34), C22(H22), C23(H23), C24(H24) 4.b Idealised Me refined as rotating group: C30(H30A,H30B,H30C), C45(H45A,H45B,H45C), C15(H15A,H15B,H15C), C47(H47A,H47B, H47C), C49(H49A,H49B,H49C) ; _shelx_res_file ; TITL 1 in P-1 1.res created by SHELXL-2018/1 at 10:46:22 on 23-Jan-2019 CELL 0.71073 13.034 15.6737 20.2719 79.875 88.908 87.011 ZERR 2 0.0006 0.0006 0.0009 0.002 0.002 0.002 LATT 1 SFAC C H Mn Mo N O P UNIT 98 78 6 24 22 98 2 EQIV $1 +X,1+Y,+Z EQIV $2 1-X,1-Y,1-Z EQIV $3 1-X,1-Y,-Z EQIV $4 1-X,-Y,1-Z EQIV $5 -1+X,+Y,+Z EQIV $6 +X,+Y,-1+Z DFIX 1.14 0.01 N10 C46 DFIX 1.38 0.01 C47 C46 SIMU 0.01 0.02 5 $c $n SIMU 0.01 0.02 5 $O ISOR 0.1 0.02 C46 C47 O49 N10 L.S. 20 PLAN 20 SIZE 0.26 0.28 0.31 TEMP 0 HTAB C7 O29_$1 HTAB C10 O4 HTAB C19 O7_$2 HTAB C32 O36_$3 HTAB C16 O30_$4 HTAB C30 O24_$2 HTAB C45 N11_$2 HTAB C45 O9_$5 HTAB C45 O12_$5 HTAB C31 O7_$3 HTAB C47 O45_$6 HTAB C47 O33 HTAB bond $H fmap 2 acta OMIT 0 2 2 OMIT -1 -1 2 REM REM REM WGHT 0.023100 27.164700 EXTI 0.000273 FVAR 0.04670 MO1 4 0.483536 0.186565 0.198169 11.00000 0.03283 0.03021 = 0.02466 -0.00789 -0.00287 -0.01004 MO10 4 0.542464 0.082212 0.371716 11.00000 0.03468 0.02248 = 0.02891 -0.00156 -0.00360 -0.00837 MO8 4 0.658413 0.194757 0.476056 11.00000 0.03760 0.03055 = 0.02064 -0.00375 -0.00356 -0.00069 MO9 4 0.354641 0.269573 0.339901 11.00000 0.02353 0.02958 = 0.03814 -0.00808 0.00358 -0.00289 MO3 4 0.588994 0.378746 0.133309 11.00000 0.03689 0.03041 = 0.02043 -0.00045 -0.00240 -0.00341 MO5 4 0.715710 0.502279 0.245790 11.00000 0.03691 0.02135 = 0.03271 -0.00340 0.00033 -0.00758 MO6 4 0.770374 0.404623 0.407514 11.00000 0.04095 0.03528 = 0.02673 -0.00955 -0.00163 -0.01619 MO2 4 0.745275 0.195501 0.177339 11.00000 0.03196 0.03851 = 0.02669 -0.01297 0.00327 0.00407 MO11 4 0.801266 0.113696 0.355759 11.00000 0.03000 0.02737 = 0.03338 -0.00267 -0.00124 0.00742 MO12 4 0.436142 0.467187 0.264056 11.00000 0.03571 0.02820 = 0.03637 0.00133 0.00398 0.00975 MO7 4 0.489016 0.391732 0.429376 11.00000 0.04105 0.03246 = 0.02874 -0.01328 0.00442 0.00508 MO4 4 0.888477 0.327755 0.274860 11.00000 0.02361 0.03546 = 0.04572 -0.01111 0.00253 -0.00663 P1 7 0.622809 0.293766 0.305891 11.00000 0.02012 0.01753 = 0.01567 -0.00476 0.00034 0.00004 MN2 3 0.694980 0.141068 0.789306 11.00000 0.03765 0.03827 = 0.03189 -0.01216 -0.00049 0.00079 MN3 3 0.063335 0.202184 -0.008196 11.00000 0.04511 0.03717 = 0.03897 -0.00260 0.00090 -0.00695 MN1 3 0.917661 0.765242 0.401575 11.00000 0.02969 0.05183 = 0.04787 -0.01163 0.00372 0.00821 O10 6 0.675828 0.446269 0.171215 11.00000 0.03322 0.03284 = 0.03199 -0.00777 0.00320 -0.00164 O15 6 0.771765 0.127004 0.259439 11.00000 0.03496 0.02936 = 0.03112 -0.00655 -0.00204 -0.00009 O26 6 0.429460 0.169689 0.375248 11.00000 0.03522 0.02970 = 0.02846 -0.00684 0.00250 -0.00266 O30 6 0.524084 0.106830 0.279931 11.00000 0.03414 0.02491 = 0.02892 -0.00499 -0.00078 -0.00348 O3 6 0.747082 0.294301 0.452813 11.00000 0.03491 0.03367 = 0.03057 -0.00526 -0.00149 -0.00570 O33 6 0.620071 0.148668 0.165742 11.00000 0.03547 0.03111 = 0.03278 -0.00779 0.00023 -0.00321 N9 5 -0.027606 0.295088 0.023113 11.00000 0.04153 0.04501 = 0.05296 0.00105 0.00031 -0.00176 O29 6 0.480562 -0.009226 0.394129 11.00000 0.04889 0.02589 = 0.04154 0.00103 -0.00230 -0.00857 O9 6 0.849920 0.440660 0.235055 11.00000 0.03338 0.03475 = 0.03393 -0.00576 0.00423 -0.00416 O21 6 0.551241 0.277753 0.467298 11.00000 0.03583 0.03152 = 0.03072 -0.00599 0.00171 -0.00364 O34 6 0.393012 0.238693 0.251663 11.00000 0.03406 0.03086 = 0.02932 -0.00443 -0.00406 -0.00354 O24 6 0.436307 0.476197 0.359723 11.00000 0.03801 0.02967 = 0.03702 -0.00756 0.00285 -0.00004 O38 6 0.479738 0.425767 0.187591 11.00000 0.03425 0.03409 = 0.03379 -0.00298 -0.00082 -0.00169 O8 6 0.575667 0.510256 0.264198 11.00000 0.03537 0.03039 = 0.03476 -0.00741 0.00364 -0.00094 O12 6 0.834683 0.278160 0.207853 11.00000 0.03375 0.03354 = 0.03340 -0.00428 -0.00047 -0.00341 O19 6 0.574734 0.106367 0.460452 11.00000 0.03759 0.03166 = 0.02788 -0.00568 -0.00008 -0.00500 O32 6 0.494086 0.285429 0.132154 11.00000 0.03522 0.03354 = 0.03283 -0.00274 -0.00174 -0.00265 O20 6 0.671580 0.169458 0.558881 11.00000 0.04561 0.04124 = 0.02507 -0.00347 -0.00405 -0.00785 O40 6 0.820412 0.150987 0.123884 11.00000 0.04466 0.05236 = 0.03571 -0.01668 0.00736 0.00700 O13 6 0.869324 0.214667 0.332925 11.00000 0.03603 0.03388 = 0.03340 -0.00581 -0.00446 -0.00303 O4 6 0.753870 0.505483 0.333253 11.00000 0.03883 0.03122 = 0.03364 -0.01041 -0.00024 -0.00559 O5 6 0.885688 0.371086 0.361550 11.00000 0.03383 0.03717 = 0.03524 -0.00696 -0.00452 -0.00497 O2 6 0.622154 0.427473 0.420096 11.00000 0.03871 0.03021 = 0.03389 -0.00778 0.00212 -0.00218 O23 6 0.369055 0.323033 0.413267 11.00000 0.03670 0.03311 = 0.03373 -0.00583 0.00576 -0.00155 N2 5 0.764175 0.750434 0.397812 11.00000 0.04152 0.03519 = 0.03881 -0.01063 0.00260 -0.00534 N8 5 0.087006 0.158089 0.092047 11.00000 0.03595 0.03883 = 0.05211 -0.00271 0.00399 0.00197 C27 1 0.704216 0.052120 0.859943 11.00000 0.05065 0.04390 = 0.04171 -0.01605 -0.00399 -0.00126 O27 6 0.334010 0.387158 0.285508 11.00000 0.03526 0.03280 = 0.03589 -0.00145 -0.00060 0.00159 O16 6 0.775463 0.128653 0.444556 11.00000 0.03441 0.03290 = 0.03227 -0.00411 -0.00491 -0.00209 O37 6 0.693177 0.300900 0.114465 11.00000 0.03611 0.03458 = 0.03157 -0.00529 0.00317 -0.00303 N4 5 0.538415 0.139017 0.786810 11.00000 0.04494 0.03763 = 0.03740 -0.01601 -0.00177 -0.00089 N1 5 0.863919 0.846449 0.463970 11.00000 0.04136 0.03945 = 0.03796 -0.00648 0.00089 -0.00822 O22 6 0.443618 0.426558 0.497670 11.00000 0.05615 0.04364 = 0.03890 -0.02150 0.01456 -0.00221 O17 6 0.679967 0.040766 0.365725 11.00000 0.03689 0.02876 = 0.03157 -0.00785 -0.00228 0.00053 O28 6 0.520619 0.336498 0.325468 11.00000 0.02954 0.02658 = 0.02836 -0.00838 0.00056 -0.00138 O11 6 1.014847 0.324478 0.260694 11.00000 0.02972 0.05052 = 0.05815 -0.00903 0.00453 -0.00604 O36 6 0.566710 0.438537 0.057433 11.00000 0.04614 0.03911 = 0.02874 0.00239 -0.00667 -0.00846 N5 5 0.652237 0.230985 0.848562 11.00000 0.04877 0.04041 = 0.03760 -0.01655 -0.00220 -0.00535 O39 6 0.366139 0.558640 0.235358 11.00000 0.04531 0.03454 = 0.04842 0.00485 0.00503 0.01395 N7 5 0.178313 0.277452 0.010214 11.00000 0.03969 0.04173 = 0.05653 0.00002 0.00611 -0.00335 O31 6 0.408857 0.125286 0.162315 11.00000 0.05029 0.04752 = 0.03830 -0.01633 -0.00961 -0.01644 O7 6 0.739824 0.602161 0.205278 11.00000 0.05460 0.02891 = 0.04427 -0.00232 0.00737 -0.01054 N6 5 0.688179 0.241929 0.711349 11.00000 0.04754 0.04390 = 0.04108 -0.01393 0.00085 -0.00306 C6 1 0.704028 0.805710 0.428499 11.00000 0.03974 0.03577 = 0.03700 -0.00584 0.00424 -0.00350 O1 6 0.821349 0.452022 0.465633 11.00000 0.05967 0.04852 = 0.04169 -0.01702 -0.00953 -0.01554 C5 1 0.760315 0.857653 0.466936 11.00000 0.04110 0.03627 = 0.03614 -0.00635 0.00481 -0.00196 O14 6 0.895878 0.036737 0.365488 11.00000 0.04163 0.03555 = 0.04849 -0.00230 -0.00341 0.01375 C7 1 0.599501 0.809403 0.422454 11.00000 0.04096 0.04039 = 0.04066 -0.00445 0.00490 -0.00416 AFIX 43 H7 2 0.559160 0.848670 0.442425 11.00000 -1.20000 AFIX 0 C4 1 0.713038 0.912448 0.506379 11.00000 0.04582 0.03741 = 0.03706 -0.00554 0.00335 -0.00310 AFIX 43 H4 2 0.641918 0.921228 0.506307 11.00000 -1.20000 AFIX 0 O35 6 0.613915 0.273254 0.235242 11.00000 0.03157 0.02739 = 0.02699 -0.00701 -0.00052 -0.00109 C11 1 0.904679 0.847101 0.327878 11.00000 0.04616 0.04662 = 0.04427 -0.00965 0.00487 -0.00558 C20 1 0.486007 0.197854 0.817798 11.00000 0.04594 0.04137 = 0.03835 -0.01463 0.00126 -0.00107 C35 1 0.199461 0.273948 0.075051 11.00000 0.04008 0.04449 = 0.05795 -0.00216 0.00151 0.00033 O25 6 0.232616 0.240503 0.347537 11.00000 0.03420 0.04909 = 0.05361 -0.00465 0.00028 -0.00496 C10 1 0.718451 0.697057 0.364634 11.00000 0.05021 0.04446 = 0.04484 -0.01218 0.00400 -0.00508 AFIX 43 H10 2 0.759384 0.658226 0.344594 11.00000 -1.20000 AFIX 0 C17 1 0.379157 0.082948 0.761141 11.00000 0.05077 0.04852 = 0.04506 -0.01493 -0.00327 -0.00812 AFIX 43 H17 2 0.344586 0.043216 0.741874 11.00000 -1.20000 AFIX 0 C38 1 0.103911 0.130888 0.229973 11.00000 0.04791 0.05517 = 0.05655 -0.00050 0.00039 0.00583 AFIX 43 H38 2 0.108440 0.123033 0.276396 11.00000 -1.20000 AFIX 0 O45 6 0.713668 -0.003576 0.903464 11.00000 0.08453 0.05472 = 0.05315 0.00069 -0.01984 -0.00391 N3 5 0.917261 0.674276 0.485075 11.00000 0.05037 0.04945 = 0.05163 -0.00496 0.00027 0.00027 C40 1 0.038571 0.094505 0.130749 11.00000 0.04042 0.04397 = 0.05594 -0.00006 0.00429 -0.00023 AFIX 43 H40 2 -0.000969 0.058955 0.110408 11.00000 -1.20000 AFIX 0 C44 1 -0.066790 0.351190 0.042531 11.00000 0.04057 0.04568 = 0.05481 0.00141 0.00224 -0.00290 C28 1 0.830844 0.149233 0.795148 11.00000 0.05167 0.05031 = 0.04878 -0.01701 -0.00135 -0.00266 C3 1 0.771830 0.953826 0.545670 11.00000 0.05771 0.03739 = 0.03542 -0.00558 0.00374 -0.00392 AFIX 43 H3 2 0.741224 0.990639 0.572459 11.00000 -1.20000 AFIX 0 C36 1 0.147342 0.207268 0.121802 11.00000 0.03953 0.04335 = 0.05373 -0.00061 0.00036 0.00159 C2 1 0.875271 0.939663 0.544395 11.00000 0.05640 0.04525 = 0.04426 -0.00843 -0.00413 -0.01115 AFIX 43 H2 2 0.916341 0.965518 0.571503 11.00000 -1.20000 AFIX 0 C29 1 0.692163 0.295943 0.667258 11.00000 0.05019 0.04359 = 0.03985 -0.01562 0.00028 -0.00155 O46 6 0.918114 0.152670 0.798995 11.00000 0.04399 0.12522 = 0.11526 -0.04469 -0.00057 -0.01042 C39 1 0.044783 0.079200 0.200265 11.00000 0.04641 0.04898 = 0.05675 0.00598 0.00638 0.00404 AFIX 43 H39 2 0.009479 0.034772 0.225971 11.00000 -1.20000 AFIX 0 C19 1 0.379098 0.201495 0.820319 11.00000 0.04803 0.04895 = 0.04622 -0.01682 0.00341 0.00059 AFIX 43 H19 2 0.343457 0.242981 0.840697 11.00000 -1.20000 AFIX 0 C32 1 0.293145 0.392130 -0.018513 11.00000 0.04540 0.04778 = 0.06710 0.00046 0.00459 -0.00377 AFIX 43 H32 2 0.324450 0.431325 -0.051613 11.00000 -1.20000 AFIX 0 O41 6 0.895193 0.897923 0.279909 11.00000 0.07061 0.07910 = 0.05768 -0.00866 0.00837 -0.01636 C16 1 0.484353 0.083696 0.759455 11.00000 0.04758 0.04302 = 0.04222 -0.01585 -0.00198 -0.00418 AFIX 43 H16 2 0.520446 0.043441 0.738065 11.00000 -1.20000 AFIX 0 C30 1 0.700354 0.364817 0.609080 11.00000 0.07036 0.04269 = 0.04736 -0.00383 0.00793 0.00437 AFIX 137 H30A 2 0.752093 0.347936 0.578902 11.00000 -1.50000 H30B 2 0.718854 0.417123 0.623404 11.00000 -1.50000 H30C 2 0.635506 0.374723 0.586639 11.00000 -1.50000 AFIX 0 O18 6 0.645941 0.208824 0.355114 11.00000 0.03054 0.02529 = 0.02647 -0.00622 -0.00005 -0.00321 C45 1 -0.118967 0.426856 0.064197 11.00000 0.05730 0.05271 = 0.05741 0.00197 0.01128 0.00069 AFIX 137 H45A 2 -0.180221 0.443114 0.038504 11.00000 -1.50000 H45B 2 -0.074058 0.474331 0.057404 11.00000 -1.50000 H45C 2 -0.136786 0.412668 0.110869 11.00000 -1.50000 AFIX 0 C37 1 0.156330 0.194363 0.190342 11.00000 0.04447 0.05175 = 0.05917 -0.00124 0.00163 0.00276 AFIX 43 H37 2 0.198283 0.228983 0.209871 11.00000 -1.20000 AFIX 0 C25 1 0.715299 0.273970 0.881062 11.00000 0.05553 0.04957 = 0.04648 -0.01622 -0.00435 -0.00371 AFIX 43 H25 2 0.785752 0.261815 0.878784 11.00000 -1.20000 AFIX 0 C18 1 0.327017 0.143156 0.792385 11.00000 0.04562 0.05537 = 0.05006 -0.01342 -0.00149 -0.00584 AFIX 43 H18 2 0.255635 0.144421 0.794644 11.00000 -1.20000 AFIX 0 C1 1 0.919403 0.887142 0.503077 11.00000 0.04688 0.04711 = 0.04551 -0.00709 0.00086 -0.00956 AFIX 43 H1 2 0.990611 0.879408 0.502111 11.00000 -1.20000 AFIX 0 C21 1 0.550033 0.251188 0.850281 11.00000 0.04753 0.04047 = 0.03742 -0.01463 0.00196 -0.00287 C43 1 0.048628 0.253188 -0.093793 11.00000 0.05289 0.05067 = 0.05787 -0.00130 -0.00023 -0.00633 O49 6 0.038544 0.286147 -0.149669 11.00000 0.15611 0.10318 = 0.05214 0.00959 -0.02494 -0.04239 C33 1 0.313717 0.389482 0.046286 11.00000 0.04355 0.04928 = 0.07162 -0.00156 -0.00330 -0.00362 AFIX 43 H33 2 0.359425 0.427471 0.058478 11.00000 -1.20000 AFIX 0 O6 6 0.709334 0.354949 0.307948 11.00000 0.02930 0.02770 = 0.02926 -0.00669 -0.00079 -0.00488 C8 1 0.554250 0.754747 0.386682 11.00000 0.04218 0.04963 = 0.04619 -0.00599 0.00196 -0.01088 AFIX 43 H8 2 0.483283 0.757711 0.381809 11.00000 -1.20000 AFIX 0 C9 1 0.613137 0.696604 0.358558 11.00000 0.05047 0.04983 = 0.04614 -0.01100 -0.00177 -0.01283 AFIX 43 H9 2 0.583514 0.657595 0.335861 11.00000 -1.20000 AFIX 0 C31 1 0.224196 0.335195 -0.035172 11.00000 0.04718 0.04832 = 0.06085 -0.00066 0.00604 -0.00128 AFIX 43 H31 2 0.209346 0.337488 -0.080158 11.00000 -1.20000 AFIX 0 O42 6 0.985760 0.635791 0.318227 11.00000 0.11020 0.09284 = 0.09751 -0.03819 0.01623 0.03213 C12 1 0.957858 0.687235 0.350616 11.00000 0.05648 0.05528 = 0.05472 -0.00955 0.00402 0.00655 C34 1 0.267601 0.330831 0.095028 11.00000 0.04588 0.04998 = 0.06473 -0.00154 -0.00562 -0.00036 AFIX 43 H34 2 0.281298 0.328967 0.140128 11.00000 -1.20000 AFIX 0 C14 1 0.907405 0.626512 0.532533 11.00000 0.05364 0.04929 = 0.05139 -0.00627 -0.00031 -0.00359 C22 1 0.510950 0.316352 0.883355 11.00000 0.05254 0.04530 = 0.04482 -0.01852 0.00329 -0.00180 AFIX 43 H22 2 0.441073 0.331864 0.882042 11.00000 -1.20000 AFIX 0 C23 1 0.576517 0.357687 0.918039 11.00000 0.06382 0.04903 = 0.04584 -0.01921 0.00179 -0.00254 AFIX 43 H23 2 0.551168 0.400338 0.941496 11.00000 -1.20000 AFIX 0 C24 1 0.679013 0.335699 0.917804 11.00000 0.06208 0.05134 = 0.04856 -0.01944 -0.00782 -0.00878 AFIX 43 H24 2 0.724053 0.361976 0.942123 11.00000 -1.20000 AFIX 0 O44 6 0.733785 0.015149 0.697748 11.00000 0.09765 0.08144 = 0.05852 -0.04164 -0.00984 0.02549 C15 1 0.891438 0.567210 0.595130 11.00000 0.07250 0.07782 = 0.07081 0.00769 -0.01124 -0.00998 AFIX 137 H15A 2 0.833610 0.533098 0.590942 11.00000 -1.50000 H15B 2 0.878471 0.599782 0.630598 11.00000 -1.50000 H15C 2 0.951688 0.529584 0.605190 11.00000 -1.50000 AFIX 0 O43 6 1.132459 0.812527 0.402448 11.00000 0.04672 0.22314 = 0.13365 -0.03582 0.00416 -0.02337 C26 1 0.718337 0.064581 0.732443 11.00000 0.05120 0.04918 = 0.04268 -0.01263 -0.00316 0.00370 C13 1 1.048900 0.790685 0.405900 11.00000 0.05276 0.06542 = 0.05566 -0.00718 0.00295 -0.00199 N11 5 0.896302 0.481265 0.902245 11.00000 0.10998 0.11950 = 0.08246 -0.00841 0.00093 -0.00592 C46 1 0.494636 0.127034 0.005791 11.00000 0.06663 0.07621 = 0.07828 0.00064 0.00542 -0.00085 C47 1 0.584499 0.084307 0.031681 11.00000 0.13464 0.16298 = 0.11386 -0.06142 0.00968 0.00895 AFIX 137 H47A 2 0.621178 0.060213 -0.002820 11.00000 -1.50000 H47B 2 0.568270 0.038522 0.067823 11.00000 -1.50000 H47C 2 0.626407 0.124535 0.048004 11.00000 -1.50000 AFIX 0 C49 1 0.886288 0.483158 0.776788 11.00000 0.07872 0.08186 = 0.06661 -0.00733 0.00242 -0.00869 AFIX 137 H49A 2 0.847656 0.534728 0.756769 11.00000 -1.50000 H49B 2 0.853526 0.433070 0.767687 11.00000 -1.50000 H49C 2 0.954690 0.483953 0.758345 11.00000 -1.50000 AFIX 0 N10 5 0.416903 0.161707 -0.007677 11.00000 0.10390 0.10295 = 0.09852 0.00621 0.00590 -0.00418 C48 1 0.890681 0.479815 0.846587 11.00000 0.07500 0.07202 = 0.06282 -0.01031 0.00025 -0.00254 O47 6 0.203005 0.071640 -0.056521 11.00000 0.11484 0.06964 = 0.08961 -0.01714 0.02999 0.00788 O48 6 -0.107921 0.093371 -0.026728 11.00000 0.10764 0.10019 = 0.08805 -0.01391 -0.01792 -0.06062 C41 1 0.150053 0.121925 -0.036068 11.00000 0.05187 0.04945 = 0.05951 -0.00167 0.00765 -0.00165 C42 1 -0.042463 0.135833 -0.018151 11.00000 0.04981 0.04786 = 0.05821 -0.00118 -0.00167 -0.00520 HKLF 4 REM 1 in P-1 REM R1 = 0.0481 for 11784 Fo > 4sig(Fo) and 0.0955 for all 17989 data REM 1132 parameters refined using 4334 restraints END WGHT 0.0231 27.1920 REM Instructions for potential hydrogen bonds HTAB C7 O29_$1 HTAB C10 O4 HTAB C19 O7_$2 HTAB C32 O36_$3 HTAB C16 O30_$4 HTAB C30 O24_$2 HTAB C45 N11_$2 HTAB C45 O9_$5 HTAB C45 O12_$5 HTAB C31 O7_$3 HTAB C47 O45_$6 HTAB C47 O33 REM Highest difference peak 1.137, deepest hole -1.314, 1-sigma level 0.157 Q1 1 0.6014 0.8277 0.4984 11.00000 0.05 1.14 Q2 1 1.0596 0.7795 0.5492 11.00000 0.05 0.99 Q3 1 0.4876 0.5024 0.2489 11.00000 0.05 0.97 Q4 1 0.3107 0.3683 0.1641 11.00000 0.05 0.97 Q5 1 0.8940 0.3192 0.3134 11.00000 0.05 0.87 Q6 1 0.3355 0.0006 0.7580 11.00000 0.05 0.86 Q7 1 0.5921 0.5895 0.3684 11.00000 0.05 0.84 Q8 1 0.7687 0.2404 0.1783 11.00000 0.05 0.82 Q9 1 0.8220 0.9523 0.5469 11.00000 0.05 0.80 Q10 1 0.4247 0.2671 0.0273 11.00000 0.05 0.79 Q11 1 0.3487 0.2901 0.3034 11.00000 0.05 0.79 Q12 1 1.0586 0.8348 0.3956 11.00000 0.05 0.79 Q13 1 0.3012 0.3861 0.0878 11.00000 0.05 0.78 Q14 1 0.7264 0.4332 0.4069 11.00000 0.05 0.77 Q15 1 0.5231 0.4545 0.9668 11.00000 0.05 0.76 Q16 1 0.3382 0.4197 -0.0714 11.00000 0.05 0.73 Q17 1 0.2386 0.3262 0.1218 11.00000 0.05 0.73 Q18 1 0.6162 0.3847 0.2518 11.00000 0.05 0.71 Q19 1 0.6585 0.0976 0.3504 11.00000 0.05 0.71 Q20 1 0.5011 0.4692 0.3477 11.00000 0.05 0.68 ; _shelx_res_checksum 59069 _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 Mo1 Mo 0.48354(5) 0.18656(4) 0.19817(3) 0.02853(14) Uani 1 1 d . . Mo10 Mo 0.54246(5) 0.08221(4) 0.37172(3) 0.02876(14) Uani 1 1 d . . Mo8 Mo 0.65841(5) 0.19476(4) 0.47606(3) 0.02968(14) Uani 1 1 d . . Mo9 Mo 0.35464(5) 0.26957(4) 0.33990(3) 0.03015(14) Uani 1 1 d . . Mo3 Mo 0.58899(5) 0.37875(4) 0.13331(3) 0.02964(14) Uani 1 1 d . . Mo5 Mo 0.71571(5) 0.50228(4) 0.24579(3) 0.03028(14) Uani 1 1 d . . Mo6 Mo 0.77037(5) 0.40462(4) 0.40751(3) 0.03330(15) Uani 1 1 d . . Mo2 Mo 0.74527(5) 0.19550(4) 0.17734(3) 0.03176(15) Uani 1 1 d . . Mo11 Mo 0.80127(5) 0.11370(4) 0.35576(3) 0.03087(14) Uani 1 1 d . . Mo12 Mo 0.43614(5) 0.46719(4) 0.26406(3) 0.03473(16) Uani 1 1 d . . Mo7 Mo 0.48902(5) 0.39173(4) 0.42938(3) 0.03343(15) Uani 1 1 d . . Mo4 Mo 0.88848(5) 0.32775(4) 0.27486(3) 0.03430(15) Uani 1 1 d . . P1 P 0.62281(12) 0.29377(10) 0.30589(8) 0.0176(3) Uani 1 1 d . . Mn2 Mn 0.69498(9) 0.14107(7) 0.78931(6) 0.0353(3) Uani 1 1 d . . Mn3 Mn 0.06333(10) 0.20218(7) -0.00820(6) 0.0408(3) Uani 1 1 d . . Mn1 Mn 0.91766(9) 0.76524(8) 0.40157(6) 0.0432(3) Uani 1 1 d . . O10 O 0.6758(4) 0.4463(3) 0.1712(2) 0.0325(9) Uani 1 1 d . U O15 O 0.7718(4) 0.1270(3) 0.2594(2) 0.0317(9) Uani 1 1 d . U O26 O 0.4295(4) 0.1697(3) 0.3752(2) 0.0309(9) Uani 1 1 d . U O30 O 0.5241(3) 0.1068(3) 0.2799(2) 0.0292(9) Uani 1 1 d . U O3 O 0.7471(4) 0.2943(3) 0.4528(2) 0.0329(9) Uani 1 1 d . U O33 O 0.6201(4) 0.1487(3) 0.1657(2) 0.0328(9) Uani 1 1 d . U N9 N -0.0276(5) 0.2951(4) 0.0231(4) 0.0477(12) Uani 1 1 d . U O29 O 0.4806(4) -0.0092(3) 0.3941(2) 0.0394(12) Uani 1 1 d . U O9 O 0.8499(4) 0.4407(3) 0.2351(2) 0.0340(9) Uani 1 1 d . U O21 O 0.5512(4) 0.2778(3) 0.4673(2) 0.0326(9) Uani 1 1 d . U O34 O 0.3930(4) 0.2387(3) 0.2517(2) 0.0314(9) Uani 1 1 d . U O24 O 0.4363(4) 0.4762(3) 0.3597(2) 0.0348(9) Uani 1 1 d . U O38 O 0.4797(4) 0.4258(3) 0.1876(2) 0.0344(9) Uani 1 1 d . U O8 O 0.5757(4) 0.5103(3) 0.2642(2) 0.0334(9) Uani 1 1 d . U O12 O 0.8347(4) 0.2782(3) 0.2079(2) 0.0337(9) Uani 1 1 d . U O19 O 0.5747(4) 0.1064(3) 0.4605(2) 0.0322(9) Uani 1 1 d . U O32 O 0.4941(4) 0.2854(3) 0.1322(2) 0.0342(9) Uani 1 1 d . U O20 O 0.6716(4) 0.1695(3) 0.5589(2) 0.0373(11) Uani 1 1 d . U O40 O 0.8204(4) 0.1510(3) 0.1239(3) 0.0436(12) Uani 1 1 d . U O13 O 0.8693(4) 0.2147(3) 0.3329(2) 0.0343(9) Uani 1 1 d . U O4 O 0.7539(4) 0.5055(3) 0.3333(2) 0.0339(9) Uani 1 1 d . U O5 O 0.8857(4) 0.3711(3) 0.3615(2) 0.0352(9) Uani 1 1 d . U O2 O 0.6222(4) 0.4275(3) 0.4201(2) 0.0340(9) Uani 1 1 d . U O23 O 0.3691(4) 0.3230(3) 0.4133(2) 0.0346(9) Uani 1 1 d . U N2 N 0.7642(5) 0.7504(4) 0.3978(3) 0.0379(11) Uani 1 1 d . U N8 N 0.0870(5) 0.1581(4) 0.0920(3) 0.0431(11) Uani 1 1 d . U C27 C 0.7042(6) 0.0521(5) 0.8599(4) 0.0444(13) Uani 1 1 d . U O27 O 0.3340(4) 0.3872(3) 0.2855(2) 0.0353(9) Uani 1 1 d . U O16 O 0.7755(4) 0.1287(3) 0.4446(2) 0.0333(9) Uani 1 1 d . U O37 O 0.6932(4) 0.3009(3) 0.1145(2) 0.0341(9) Uani 1 1 d . U N4 N 0.5384(5) 0.1390(4) 0.7868(3) 0.0389(11) Uani 1 1 d . U N1 N 0.8639(5) 0.8464(4) 0.4640(3) 0.0394(11) Uani 1 1 d . U O22 O 0.4436(4) 0.4266(3) 0.4977(3) 0.0447(13) Uani 1 1 d . U O17 O 0.6800(4) 0.0408(3) 0.3657(2) 0.0321(9) Uani 1 1 d . U O28 O 0.5206(3) 0.3365(3) 0.3255(2) 0.0277(8) Uani 1 1 d . U O11 O 1.0148(4) 0.3245(3) 0.2607(3) 0.0461(13) Uani 1 1 d . U O36 O 0.5667(4) 0.4385(3) 0.0574(2) 0.0387(12) Uani 1 1 d . U N5 N 0.6522(5) 0.2310(4) 0.8486(3) 0.0410(11) Uani 1 1 d . U O39 O 0.3661(4) 0.5586(3) 0.2354(3) 0.0449(13) Uani 1 1 d . U N7 N 0.1783(5) 0.2775(4) 0.0102(4) 0.0471(11) Uani 1 1 d . U O31 O 0.4089(4) 0.1253(3) 0.1623(3) 0.0437(12) Uani 1 1 d . U O7 O 0.7398(4) 0.6022(3) 0.2053(3) 0.0429(12) Uani 1 1 d . U N6 N 0.6882(5) 0.2419(4) 0.7113(3) 0.0434(11) Uani 1 1 d . U C6 C 0.7040(6) 0.8057(5) 0.4285(4) 0.0376(12) Uani 1 1 d . U O1 O 0.8213(4) 0.4520(3) 0.4656(3) 0.0483(13) Uani 1 1 d . U C5 C 0.7603(6) 0.8577(5) 0.4669(4) 0.0379(12) Uani 1 1 d . U O14 O 0.8959(4) 0.0367(3) 0.3655(3) 0.0430(12) Uani 1 1 d . U C7 C 0.5995(6) 0.8094(5) 0.4225(4) 0.0410(13) Uani 1 1 d . U H7 H 0.559160 0.848670 0.442425 0.049 Uiso 1 1 calc R . C4 C 0.7130(6) 0.9124(5) 0.5064(4) 0.0402(13) Uani 1 1 d . U H4 H 0.641918 0.921228 0.506307 0.048 Uiso 1 1 calc R . O35 O 0.6139(3) 0.2733(3) 0.2352(2) 0.0284(8) Uani 1 1 d . U C11 C 0.9047(6) 0.8471(5) 0.3279(4) 0.0454(13) Uani 1 1 d . U C20 C 0.4860(6) 0.1979(5) 0.8178(4) 0.0410(12) Uani 1 1 d . U C35 C 0.1995(6) 0.2739(5) 0.0751(5) 0.0484(12) Uani 1 1 d . U O25 O 0.2326(4) 0.2405(3) 0.3475(3) 0.0461(13) Uani 1 1 d . U C10 C 0.7185(6) 0.6971(5) 0.3646(4) 0.0459(13) Uani 1 1 d . U H10 H 0.759384 0.658226 0.344594 0.055 Uiso 1 1 calc R . C17 C 0.3792(6) 0.0829(5) 0.7611(4) 0.0471(14) Uani 1 1 d . U H17 H 0.344586 0.043216 0.741874 0.056 Uiso 1 1 calc R . C38 C 0.1039(7) 0.1309(6) 0.2300(5) 0.0546(16) Uani 1 1 d . U H38 H 0.108440 0.123033 0.276396 0.066 Uiso 1 1 calc R . O45 O 0.7137(5) -0.0036(4) 0.9035(3) 0.0651(17) Uani 1 1 d . U N3 N 0.9173(5) 0.6743(4) 0.4851(4) 0.0511(12) Uani 1 1 d . U C40 C 0.0386(6) 0.0945(5) 0.1307(4) 0.0480(13) Uani 1 1 d . U H40 H -0.000969 0.058955 0.110408 0.058 Uiso 1 1 calc R . C44 C -0.0668(6) 0.3512(5) 0.0425(4) 0.0483(13) Uani 1 1 d . U C28 C 0.8308(7) 0.1492(5) 0.7951(4) 0.0492(14) Uani 1 1 d . U C3 C 0.7718(7) 0.9538(5) 0.5457(4) 0.0436(14) Uani 1 1 d . U H3 H 0.741224 0.990639 0.572459 0.052 Uiso 1 1 calc R . C36 C 0.1473(6) 0.2073(5) 0.1218(4) 0.0466(13) Uani 1 1 d . U C2 C 0.8753(7) 0.9397(5) 0.5444(4) 0.0482(14) Uani 1 1 d . U H2 H 0.916341 0.965518 0.571503 0.058 Uiso 1 1 calc R . C29 C 0.6922(6) 0.2959(5) 0.6673(4) 0.0436(13) Uani 1 1 d . U O46 O 0.9181(5) 0.1527(5) 0.7990(4) 0.092(2) Uani 1 1 d . U C39 C 0.0448(7) 0.0792(6) 0.2003(4) 0.0529(15) Uani 1 1 d . U H39 H 0.009479 0.034772 0.225971 0.063 Uiso 1 1 calc R . C19 C 0.3791(6) 0.2015(5) 0.8203(4) 0.0469(13) Uani 1 1 d . U H19 H 0.343457 0.242981 0.840697 0.056 Uiso 1 1 calc R . C32 C 0.2931(7) 0.3921(5) -0.0185(5) 0.0547(14) Uani 1 1 d . U H32 H 0.324450 0.431325 -0.051613 0.066 Uiso 1 1 calc R . O41 O 0.8952(5) 0.8979(4) 0.2799(3) 0.0692(18) Uani 1 1 d . U C16 C 0.4844(6) 0.0837(5) 0.7595(4) 0.0432(13) Uani 1 1 d . U H16 H 0.520446 0.043441 0.738065 0.052 Uiso 1 1 calc R . C30 C 0.7004(7) 0.3648(5) 0.6091(4) 0.054(2) Uani 1 1 d . U H30A H 0.752093 0.347936 0.578902 0.081 Uiso 1 1 calc GR . H30B H 0.718854 0.417123 0.623404 0.081 Uiso 1 1 calc GR . H30C H 0.635506 0.374723 0.586639 0.081 Uiso 1 1 calc GR . O18 O 0.6459(3) 0.2088(3) 0.3551(2) 0.0272(8) Uani 1 1 d . U C45 C -0.1190(7) 0.4269(5) 0.0642(5) 0.057(2) Uani 1 1 d . U H45A H -0.180221 0.443114 0.038504 0.086 Uiso 1 1 calc GR . H45B H -0.074058 0.474331 0.057404 0.086 Uiso 1 1 calc GR . H45C H -0.136786 0.412668 0.110869 0.086 Uiso 1 1 calc GR . C37 C 0.1563(7) 0.1944(6) 0.1903(5) 0.0530(14) Uani 1 1 d . U H37 H 0.198283 0.228983 0.209871 0.064 Uiso 1 1 calc R . C25 C 0.7153(7) 0.2740(5) 0.8811(4) 0.0495(13) Uani 1 1 d . U H25 H 0.785752 0.261815 0.878784 0.059 Uiso 1 1 calc R . C18 C 0.3270(7) 0.1432(5) 0.7924(4) 0.0497(15) Uani 1 1 d . U H18 H 0.255635 0.144421 0.794644 0.060 Uiso 1 1 calc R . C1 C 0.9194(7) 0.8871(5) 0.5031(4) 0.0464(13) Uani 1 1 d . U H1 H 0.990611 0.879408 0.502111 0.056 Uiso 1 1 calc R . C21 C 0.5500(6) 0.2512(5) 0.8503(4) 0.0409(12) Uani 1 1 d . U C43 C 0.0486(7) 0.2532(6) -0.0938(5) 0.0547(15) Uani 1 1 d . U O49 O 0.0385(7) 0.2861(5) -0.1497(4) 0.105(3) Uani 1 1 d . U C33 C 0.3137(7) 0.3895(6) 0.0463(5) 0.0558(15) Uani 1 1 d . U H33 H 0.359425 0.427471 0.058478 0.067 Uiso 1 1 calc R . O6 O 0.7093(3) 0.3549(3) 0.3079(2) 0.0284(8) Uani 1 1 d . U C8 C 0.5543(7) 0.7547(5) 0.3867(4) 0.0460(14) Uani 1 1 d . U H8 H 0.483283 0.757711 0.381809 0.055 Uiso 1 1 calc R . C9 C 0.6131(7) 0.6966(5) 0.3586(4) 0.0481(14) Uani 1 1 d . U H9 H 0.583514 0.657595 0.335861 0.058 Uiso 1 1 calc R . C31 C 0.2242(7) 0.3352(5) -0.0352(5) 0.0533(14) Uani 1 1 d . U H31 H 0.209346 0.337488 -0.080158 0.064 Uiso 1 1 calc R . O42 O 0.9858(7) 0.6358(5) 0.3182(4) 0.099(2) Uani 1 1 d . U C12 C 0.9579(7) 0.6872(6) 0.3506(5) 0.0559(15) Uani 1 1 d . U C34 C 0.2676(7) 0.3308(5) 0.0950(5) 0.0546(14) Uani 1 1 d . U H34 H 0.281298 0.328967 0.140128 0.065 Uiso 1 1 calc R . C14 C 0.9074(7) 0.6265(6) 0.5325(5) 0.0517(14) Uani 1 1 d . U C22 C 0.5110(7) 0.3164(5) 0.8834(4) 0.0463(13) Uani 1 1 d . U H22 H 0.441073 0.331864 0.882042 0.056 Uiso 1 1 calc R . C23 C 0.5765(7) 0.3577(5) 0.9180(4) 0.0516(15) Uani 1 1 d . U H23 H 0.551168 0.400338 0.941496 0.062 Uiso 1 1 calc R . C24 C 0.6790(7) 0.3357(5) 0.9178(4) 0.0524(14) Uani 1 1 d . U H24 H 0.724053 0.361976 0.942123 0.063 Uiso 1 1 calc R . O44 O 0.7338(6) 0.0151(4) 0.6977(3) 0.077(2) Uani 1 1 d . U C15 C 0.8914(8) 0.5672(7) 0.5951(5) 0.076(3) Uani 1 1 d . U H15A H 0.833610 0.533098 0.590942 0.114 Uiso 1 1 calc GR . H15B H 0.878471 0.599782 0.630598 0.114 Uiso 1 1 calc GR . H15C H 0.951688 0.529584 0.605190 0.114 Uiso 1 1 calc GR . O43 O 1.1325(6) 0.8125(8) 0.4024(5) 0.133(3) Uani 1 1 d . U C26 C 0.7183(7) 0.0646(5) 0.7324(4) 0.0473(14) Uani 1 1 d . U C13 C 1.0489(8) 0.7907(6) 0.4059(5) 0.0584(15) Uani 1 1 d . U N11 N 0.8963(9) 0.4813(7) 0.9022(6) 0.105(3) Uani 1 1 d . U C46 C 0.4946(8) 0.1270(7) 0.0058(6) 0.0756(19) Uani 1 1 d D U C47 C 0.5845(10) 0.0843(10) 0.0317(7) 0.133(5) Uani 1 1 d D U H47A H 0.621178 0.060213 -0.002820 0.200 Uiso 1 1 calc GR . H47B H 0.568270 0.038522 0.067823 0.200 Uiso 1 1 calc GR . H47C H 0.626407 0.124535 0.048004 0.200 Uiso 1 1 calc GR . C49 C 0.8863(8) 0.4832(7) 0.7768(5) 0.076(3) Uani 1 1 d . U H49A H 0.847656 0.534728 0.756769 0.114 Uiso 1 1 calc GR . H49B H 0.853526 0.433070 0.767687 0.114 Uiso 1 1 calc GR . H49C H 0.954690 0.483953 0.758345 0.114 Uiso 1 1 calc GR . N10 N 0.4169(8) 0.1617(7) -0.0077(5) 0.105(3) Uani 1 1 d D U C48 C 0.8907(8) 0.4798(7) 0.8466(6) 0.070(2) Uani 1 1 d . U O47 O 0.2030(7) 0.0716(5) -0.0565(4) 0.092(2) Uani 1 1 d . U O48 O -0.1079(6) 0.0934(5) -0.0267(4) 0.097(3) Uani 1 1 d . U C41 C 0.1501(7) 0.1219(6) -0.0361(5) 0.0547(13) Uani 1 1 d . U C42 C -0.0425(7) 0.1358(6) -0.0182(5) 0.0528(15) Uani 1 1 d . 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 Mo1 0.0328(3) 0.0302(3) 0.0247(3) -0.0079(2) -0.0029(3) -0.0100(2) Mo10 0.0347(3) 0.0225(3) 0.0289(3) -0.0016(2) -0.0036(3) -0.0084(2) Mo8 0.0376(4) 0.0305(3) 0.0206(3) -0.0037(2) -0.0036(3) -0.0007(3) Mo9 0.0235(3) 0.0296(3) 0.0381(4) -0.0081(3) 0.0036(3) -0.0029(2) Mo3 0.0369(4) 0.0304(3) 0.0204(3) -0.0005(2) -0.0024(3) -0.0034(3) Mo5 0.0369(4) 0.0214(3) 0.0327(3) -0.0034(2) 0.0003(3) -0.0076(2) Mo6 0.0409(4) 0.0353(3) 0.0267(3) -0.0096(3) -0.0016(3) -0.0162(3) Mo2 0.0320(3) 0.0385(3) 0.0267(3) -0.0130(3) 0.0033(3) 0.0041(3) Mo11 0.0300(3) 0.0274(3) 0.0334(3) -0.0027(2) -0.0012(3) 0.0074(2) Mo12 0.0357(4) 0.0282(3) 0.0364(4) 0.0013(3) 0.0040(3) 0.0098(3) Mo7 0.0411(4) 0.0325(3) 0.0287(3) -0.0133(3) 0.0044(3) 0.0051(3) Mo4 0.0236(3) 0.0355(3) 0.0457(4) -0.0111(3) 0.0025(3) -0.0066(3) P1 0.0201(8) 0.0175(7) 0.0157(7) -0.0048(6) 0.0003(6) 0.0000(6) Mn2 0.0377(7) 0.0383(6) 0.0319(6) -0.0122(5) -0.0005(5) 0.0008(5) Mn3 0.0451(7) 0.0372(6) 0.0390(7) -0.0026(5) 0.0009(6) -0.0070(5) Mn1 0.0297(6) 0.0518(7) 0.0479(7) -0.0116(6) 0.0037(5) 0.0082(5) O10 0.0332(19) 0.0328(18) 0.0320(19) -0.0078(16) 0.0032(17) -0.0016(16) O15 0.0350(19) 0.0294(18) 0.0311(19) -0.0065(16) -0.0020(17) -0.0001(16) O26 0.0352(19) 0.0297(18) 0.0285(18) -0.0068(16) 0.0025(17) -0.0027(16) O30 0.0341(19) 0.0249(17) 0.0289(18) -0.0050(15) -0.0008(16) -0.0035(16) O3 0.0349(19) 0.0337(18) 0.0306(19) -0.0053(16) -0.0015(17) -0.0057(16) O33 0.0355(19) 0.0311(18) 0.0328(19) -0.0078(16) 0.0002(17) -0.0032(16) N9 0.042(2) 0.045(2) 0.053(2) 0.001(2) 0.000(2) -0.002(2) O29 0.049(3) 0.026(2) 0.042(3) 0.001(2) -0.002(2) -0.009(2) O9 0.0334(19) 0.0347(19) 0.0339(19) -0.0058(16) 0.0042(17) -0.0042(17) O21 0.0358(19) 0.0315(18) 0.0307(18) -0.0060(16) 0.0017(17) -0.0036(16) O34 0.0341(19) 0.0309(18) 0.0293(18) -0.0044(16) -0.0041(17) -0.0035(16) O24 0.038(2) 0.0297(18) 0.0370(19) -0.0076(16) 0.0028(17) 0.0000(17) O38 0.0343(19) 0.0341(18) 0.0338(19) -0.0030(16) -0.0008(17) -0.0017(17) O8 0.0354(19) 0.0304(18) 0.0348(19) -0.0074(16) 0.0036(17) -0.0009(16) O12 0.0338(19) 0.0335(18) 0.0334(19) -0.0043(16) -0.0005(17) -0.0034(16) O19 0.0376(19) 0.0317(18) 0.0279(18) -0.0057(16) -0.0001(17) -0.0050(17) O32 0.0352(19) 0.0335(18) 0.0328(19) -0.0027(16) -0.0017(17) -0.0026(17) O20 0.046(3) 0.041(3) 0.025(2) -0.003(2) -0.004(2) -0.008(2) O40 0.045(3) 0.052(3) 0.036(3) -0.017(2) 0.007(2) 0.007(2) O13 0.0360(19) 0.0339(18) 0.0334(19) -0.0058(16) -0.0045(17) -0.0030(17) O4 0.039(2) 0.0312(18) 0.0336(19) -0.0104(16) -0.0002(17) -0.0056(17) O5 0.0338(19) 0.0372(18) 0.0352(19) -0.0070(16) -0.0045(17) -0.0050(17) O2 0.039(2) 0.0302(18) 0.0339(19) -0.0078(16) 0.0021(17) -0.0022(17) O23 0.037(2) 0.0331(18) 0.0337(19) -0.0058(16) 0.0058(17) -0.0015(17) N2 0.042(2) 0.035(2) 0.039(2) -0.0106(19) 0.003(2) -0.0053(19) N8 0.036(2) 0.039(2) 0.052(2) -0.003(2) 0.004(2) 0.0020(19) C27 0.051(3) 0.044(2) 0.042(2) -0.016(2) -0.004(2) -0.001(2) O27 0.035(2) 0.0328(18) 0.0359(19) -0.0015(17) -0.0006(17) 0.0016(17) O16 0.0344(19) 0.0329(18) 0.0323(19) -0.0041(16) -0.0049(17) -0.0021(16) O37 0.0361(19) 0.0346(19) 0.0316(19) -0.0053(16) 0.0032(17) -0.0030(17) N4 0.045(2) 0.038(2) 0.037(2) -0.0160(19) -0.002(2) -0.001(2) N1 0.041(2) 0.039(2) 0.038(2) -0.0065(19) 0.001(2) -0.008(2) O22 0.056(3) 0.044(3) 0.039(3) -0.022(2) 0.015(2) -0.002(2) O17 0.0369(19) 0.0288(18) 0.0316(19) -0.0079(16) -0.0023(17) 0.0005(16) O28 0.0295(16) 0.0266(15) 0.0284(15) -0.0084(13) 0.0006(14) -0.0014(14) O11 0.030(3) 0.051(3) 0.058(3) -0.009(3) 0.005(2) -0.006(2) O36 0.046(3) 0.039(3) 0.029(2) 0.002(2) -0.007(2) -0.008(2) N5 0.049(2) 0.040(2) 0.038(2) -0.0165(19) -0.002(2) -0.005(2) O39 0.045(3) 0.035(3) 0.048(3) 0.005(2) 0.005(2) 0.014(2) N7 0.040(2) 0.042(2) 0.057(2) 0.000(2) 0.006(2) -0.003(2) O31 0.050(3) 0.048(3) 0.038(3) -0.016(2) -0.010(2) -0.016(2) O7 0.055(3) 0.029(2) 0.044(3) -0.002(2) 0.007(2) -0.011(2) N6 0.048(2) 0.044(2) 0.041(2) -0.014(2) 0.001(2) -0.003(2) C6 0.040(2) 0.036(2) 0.037(2) -0.006(2) 0.004(2) -0.003(2) O1 0.060(3) 0.049(3) 0.042(3) -0.017(2) -0.010(3) -0.016(2) C5 0.041(2) 0.036(2) 0.036(2) -0.006(2) 0.005(2) -0.002(2) O14 0.042(3) 0.036(3) 0.048(3) -0.002(2) -0.003(2) 0.014(2) C7 0.041(3) 0.040(2) 0.041(3) -0.004(2) 0.005(2) -0.004(2) C4 0.046(3) 0.037(2) 0.037(2) -0.006(2) 0.003(2) -0.003(2) O35 0.0316(16) 0.0274(15) 0.0270(15) -0.0070(14) -0.0005(14) -0.0011(14) C11 0.046(2) 0.047(2) 0.044(2) -0.010(2) 0.005(2) -0.006(2) C20 0.046(2) 0.041(2) 0.038(2) -0.015(2) 0.001(2) -0.001(2) C35 0.040(2) 0.044(2) 0.058(2) -0.002(2) 0.002(2) 0.000(2) O25 0.034(3) 0.049(3) 0.054(3) -0.005(2) 0.000(2) -0.005(2) C10 0.050(3) 0.044(2) 0.045(3) -0.012(2) 0.004(2) -0.005(2) C17 0.051(3) 0.049(3) 0.045(3) -0.015(2) -0.003(3) -0.008(3) C38 0.048(3) 0.055(3) 0.057(3) 0.000(3) 0.000(3) 0.006(3) O45 0.085(5) 0.055(4) 0.053(4) 0.001(3) -0.020(3) -0.004(3) N3 0.050(2) 0.049(2) 0.052(2) -0.005(2) 0.000(2) 0.000(2) C40 0.040(3) 0.044(3) 0.056(3) 0.000(2) 0.004(2) 0.000(2) C44 0.041(3) 0.046(3) 0.055(3) 0.001(2) 0.002(2) -0.003(2) C28 0.052(3) 0.050(3) 0.049(3) -0.017(2) -0.001(3) -0.003(3) C3 0.058(3) 0.037(3) 0.035(3) -0.006(2) 0.004(3) -0.004(3) C36 0.040(2) 0.043(2) 0.054(2) -0.001(2) 0.000(2) 0.002(2) C2 0.056(3) 0.045(3) 0.044(3) -0.008(2) -0.004(3) -0.011(3) C29 0.050(3) 0.044(3) 0.040(3) -0.016(2) 0.000(2) -0.002(2) O46 0.044(4) 0.125(6) 0.115(6) -0.045(5) -0.001(4) -0.010(4) C39 0.046(3) 0.049(3) 0.057(3) 0.006(3) 0.006(3) 0.004(3) C19 0.048(3) 0.049(3) 0.046(3) -0.017(2) 0.003(2) 0.001(2) C32 0.045(3) 0.048(3) 0.067(3) 0.000(3) 0.005(3) -0.004(2) O41 0.071(4) 0.079(4) 0.058(4) -0.009(4) 0.008(3) -0.016(4) C16 0.048(3) 0.043(2) 0.042(3) -0.016(2) -0.002(2) -0.004(2) C30 0.070(5) 0.043(4) 0.047(4) -0.004(3) 0.008(4) 0.004(4) O18 0.0305(16) 0.0253(15) 0.0265(15) -0.0062(13) -0.0001(14) -0.0032(14) C45 0.057(5) 0.053(4) 0.057(5) 0.002(4) 0.011(4) 0.001(4) C37 0.044(3) 0.052(3) 0.059(3) -0.001(2) 0.002(2) 0.003(2) C25 0.056(3) 0.050(2) 0.046(2) -0.016(2) -0.004(2) -0.004(2) C18 0.046(3) 0.055(3) 0.050(3) -0.013(3) -0.001(3) -0.006(3) C1 0.047(3) 0.047(3) 0.046(3) -0.007(2) 0.001(2) -0.010(2) C21 0.048(2) 0.040(2) 0.037(2) -0.015(2) 0.002(2) -0.003(2) C43 0.053(3) 0.051(3) 0.058(3) -0.001(3) 0.000(3) -0.006(3) O49 0.156(7) 0.103(6) 0.052(4) 0.010(4) -0.025(5) -0.042(5) C33 0.044(3) 0.049(3) 0.072(3) -0.002(3) -0.003(3) -0.004(3) O6 0.0293(16) 0.0277(15) 0.0293(16) -0.0067(14) -0.0008(14) -0.0049(14) C8 0.042(3) 0.050(3) 0.046(3) -0.006(3) 0.002(3) -0.011(3) C9 0.050(3) 0.050(3) 0.046(3) -0.011(2) -0.002(3) -0.013(3) C31 0.047(3) 0.048(3) 0.061(3) -0.001(2) 0.006(2) -0.001(2) O42 0.110(5) 0.093(5) 0.098(5) -0.038(4) 0.016(4) 0.032(4) C12 0.056(3) 0.055(3) 0.055(3) -0.010(3) 0.004(3) 0.007(3) C34 0.046(3) 0.050(3) 0.065(3) -0.002(2) -0.006(2) 0.000(2) C14 0.054(3) 0.049(3) 0.051(3) -0.006(2) 0.000(3) -0.004(2) C22 0.053(3) 0.045(2) 0.045(3) -0.019(2) 0.003(2) -0.002(2) C23 0.064(3) 0.049(3) 0.046(3) -0.019(3) 0.002(3) -0.003(3) C24 0.062(3) 0.051(3) 0.049(3) -0.019(2) -0.008(3) -0.009(3) O44 0.098(5) 0.081(4) 0.059(4) -0.042(4) -0.010(4) 0.025(4) C15 0.072(6) 0.078(5) 0.071(5) 0.008(5) -0.011(5) -0.010(5) O43 0.047(5) 0.223(9) 0.134(7) -0.036(7) 0.004(5) -0.023(6) C26 0.051(3) 0.049(3) 0.043(3) -0.013(2) -0.003(3) 0.004(2) C13 0.053(3) 0.065(3) 0.056(3) -0.007(3) 0.003(3) -0.002(3) N11 0.110(6) 0.120(6) 0.082(6) -0.008(5) 0.001(6) -0.006(5) C46 0.067(4) 0.076(3) 0.078(4) 0.001(3) 0.005(3) -0.001(3) C47 0.135(9) 0.163(9) 0.114(8) -0.061(8) 0.010(8) 0.009(8) C49 0.079(5) 0.082(5) 0.067(5) -0.007(5) 0.002(5) -0.009(5) N10 0.104(5) 0.103(5) 0.099(5) 0.006(4) 0.006(5) -0.004(4) C48 0.075(4) 0.072(4) 0.063(4) -0.010(4) 0.000(4) -0.003(4) O47 0.115(6) 0.070(5) 0.090(5) -0.017(4) 0.030(5) 0.008(4) O48 0.108(6) 0.100(5) 0.088(5) -0.014(4) -0.018(5) -0.061(5) C41 0.052(3) 0.049(2) 0.060(3) -0.002(2) 0.008(2) -0.002(2) C42 0.050(3) 0.048(3) 0.058(3) -0.001(3) -0.002(3) -0.005(3) 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' Mn Mn 0.3368 0.7283 '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' P P 0.1023 0.0942 '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 O30 Mo1 O33 82.86(19) O30 Mo1 O35 81.99(16) O33 Mo1 O35 71.12(17) O34 Mo1 O30 86.41(19) O34 Mo1 O33 156.06(19) O34 Mo1 O32 95.0(2) O34 Mo1 O35 86.25(17) O32 Mo1 O30 154.9(2) O32 Mo1 O33 86.0(2) O32 Mo1 O35 73.12(18) O31 Mo1 O30 101.3(2) O31 Mo1 O33 99.9(2) O31 Mo1 O34 103.2(2) O31 Mo1 O32 102.7(2) O31 Mo1 O35 170.1(2) O26 Mo10 O18 82.67(17) O30 Mo10 O26 85.11(19) O30 Mo10 O19 156.40(18) O30 Mo10 O17 94.4(2) O30 Mo10 O18 85.49(17) O29 Mo10 O26 100.8(2) O29 Mo10 O30 102.7(2) O29 Mo10 O19 99.8(2) O29 Mo10 O17 102.5(2) O29 Mo10 O18 171.3(2) O19 Mo10 O26 83.78(19) O19 Mo10 O18 72.49(17) O17 Mo10 O26 156.24(19) O17 Mo10 O19 87.6(2) O17 Mo10 O18 73.62(17) O3 Mo8 O18 83.20(17) O21 Mo8 O3 85.0(2) O21 Mo8 O19 93.5(2) O21 Mo8 O16 155.3(2) O21 Mo8 O18 84.63(18) O19 Mo8 O3 156.87(19) O19 Mo8 O16 87.8(2) O19 Mo8 O18 73.69(17) O20 Mo8 O3 102.2(2) O20 Mo8 O21 102.4(2) O20 Mo8 O19 100.7(2) O20 Mo8 O16 101.6(2) O20 Mo8 O18 171.4(2) O16 Mo8 O3 84.18(19) O16 Mo8 O18 72.05(17) O26 Mo9 O34 85.23(19) O26 Mo9 O23 95.2(2) O26 Mo9 O27 155.1(2) O26 Mo9 O28 85.26(17) O34 Mo9 O27 82.49(19) O34 Mo9 O28 81.82(17) O23 Mo9 O34 155.7(2) O23 Mo9 O27 87.4(2) O23 Mo9 O28 73.98(18) O27 Mo9 O28 71.65(17) O25 Mo9 O26 103.9(2) O25 Mo9 O34 101.1(2) O25 Mo9 O23 102.4(2) O25 Mo9 O27 99.7(2) O25 Mo9 O28 170.6(2) O10 Mo3 O38 85.5(2) O10 Mo3 O32 156.4(2) O10 Mo3 O37 94.5(2) O10 Mo3 O35 85.71(18) O38 Mo3 O35 82.48(17) O32 Mo3 O38 83.98(19) O32 Mo3 O35 71.97(17) O37 Mo3 O38 156.3(2) O37 Mo3 O32 86.9(2) O37 Mo3 O35 73.88(17) O36 Mo3 O10 102.6(2) O36 Mo3 O38 101.4(2) O36 Mo3 O32 100.2(2) O36 Mo3 O37 101.8(2) O36 Mo3 O35 171.1(2) O10 Mo5 O9 83.28(19) O10 Mo5 O6 82.30(17) O9 Mo5 O6 71.60(17) O8 Mo5 O10 85.1(2) O8 Mo5 O9 155.14(19) O8 Mo5 O4 94.3(2) O8 Mo5 O6 85.13(17) O4 Mo5 O10 155.33(19) O4 Mo5 O9 87.4(2) O4 Mo5 O6 73.08(17) O7 Mo5 O10 101.2(2) O7 Mo5 O9 100.5(2) O7 Mo5 O8 103.3(2) O7 Mo5 O4 102.9(2) O7 Mo5 O6 171.1(2) O3 Mo6 O4 155.4(2) O3 Mo6 O5 95.0(2) O3 Mo6 O2 85.0(2) O3 Mo6 O6 86.14(17) O4 Mo6 O6 70.83(16) O5 Mo6 O4 86.6(2) O5 Mo6 O2 154.4(2) O5 Mo6 O6 73.03(18) O2 Mo6 O4 83.17(19) O2 Mo6 O6 81.45(17) O1 Mo6 O3 103.3(2) O1 Mo6 O4 100.3(2) O1 Mo6 O5 102.3(2) O1 Mo6 O2 102.6(2) O1 Mo6 O6 169.9(2) O15 Mo2 O33 95.2(2) O15 Mo2 O12 85.2(2) O15 Mo2 O37 156.16(19) O15 Mo2 O35 86.70(18) O33 Mo2 O12 154.6(2) O33 Mo2 O37 86.6(2) O33 Mo2 O35 72.70(17) O12 Mo2 O37 83.17(19) O12 Mo2 O35 81.98(17) O40 Mo2 O15 104.3(2) O40 Mo2 O33 101.4(2) O40 Mo2 O12 103.1(2) O40 Mo2 O37 98.6(2) O40 Mo2 O35 168.1(2) O37 Mo2 O35 71.13(17) O15 Mo11 O17 83.57(19) O15 Mo11 O18 82.54(17) O13 Mo11 O15 85.6(2) O13 Mo11 O16 94.4(2) O13 Mo11 O17 155.5(2) O13 Mo11 O18 85.36(18) O16 Mo11 O15 155.3(2) O16 Mo11 O17 86.6(2) O16 Mo11 O18 72.83(17) O17 Mo11 O18 71.55(16) O14 Mo11 O15 102.3(2) O14 Mo11 O13 103.5(2) O14 Mo11 O16 101.8(2) O14 Mo11 O17 100.2(2) O14 Mo11 O18 170.1(2) O24 Mo12 O8 83.9(2) O24 Mo12 O28 71.58(17) O38 Mo12 O24 156.0(2) O38 Mo12 O8 85.1(2) O38 Mo12 O27 94.5(2) O38 Mo12 O28 85.85(18) O8 Mo12 O28 82.10(17) O27 Mo12 O24 87.1(2) O27 Mo12 O8 155.9(2) O27 Mo12 O28 73.84(17) O39 Mo12 O24 98.6(2) O39 Mo12 O38 104.5(2) O39 Mo12 O8 101.8(2) O39 Mo12 O27 101.6(2) O39 Mo12 O28 169.1(2) O21 Mo7 O23 83.66(19) O21 Mo7 O28 81.50(17) O24 Mo7 O21 154.2(2) O24 Mo7 O23 85.8(2) O24 Mo7 O28 72.82(17) O2 Mo7 O21 85.5(2) O2 Mo7 O24 95.2(2) O2 Mo7 O23 156.47(19) O2 Mo7 O28 86.05(18) O23 Mo7 O28 71.73(17) O22 Mo7 O21 101.7(2) O22 Mo7 O24 103.0(2) O22 Mo7 O2 104.8(2) O22 Mo7 O23 97.9(2) O22 Mo7 O28 168.9(2) O9 Mo4 O13 155.1(2) O9 Mo4 O5 86.7(2) O9 Mo4 O6 72.95(17) O12 Mo4 O9 94.3(2) O12 Mo4 O13 85.6(2) O12 Mo4 O5 155.3(2) O12 Mo4 O6 85.80(18) O13 Mo4 O5 83.39(19) O13 Mo4 O6 82.27(17) O5 Mo4 O6 70.85(17) O11 Mo4 O9 101.9(2) O11 Mo4 O12 104.6(2) O11 Mo4 O13 102.2(2) O11 Mo4 O5 99.3(2) O11 Mo4 O6 168.8(2) O28 P1 O18 109.6(2) O35 P1 O28 109.0(3) O35 P1 O18 109.0(2) O6 P1 O28 109.8(2) O6 P1 O35 110.0(3) O6 P1 O18 109.4(3) C27 Mn2 N4 92.7(3) C27 Mn2 N5 93.3(3) C27 Mn2 N6 178.4(3) N4 Mn2 N5 78.8(2) N6 Mn2 N4 88.6(3) N6 Mn2 N5 86.1(3) C28 Mn2 C27 87.7(4) C28 Mn2 N4 175.7(3) C28 Mn2 N5 96.9(3) C28 Mn2 N6 90.8(3) C28 Mn2 C26 89.1(4) C26 Mn2 C27 89.8(4) C26 Mn2 N4 95.2(3) C26 Mn2 N5 173.4(3) C26 Mn2 N6 91.0(3) N9 Mn3 N8 84.7(3) N9 Mn3 N7 83.6(3) N7 Mn3 N8 78.9(3) C43 Mn3 N9 91.5(4) C43 Mn3 N8 172.8(3) C43 Mn3 N7 94.7(3) C43 Mn3 C41 88.5(4) C43 Mn3 C42 88.7(4) C41 Mn3 N9 177.3(4) C41 Mn3 N8 95.1(3) C41 Mn3 N7 93.7(4) C41 Mn3 C42 89.1(4) C42 Mn3 N9 93.6(3) C42 Mn3 N8 97.5(3) C42 Mn3 N7 175.6(4) N2 Mn1 N1 79.3(2) C11 Mn1 N2 88.1(3) C11 Mn1 N1 93.6(3) C11 Mn1 N3 174.4(3) N3 Mn1 N2 86.5(3) N3 Mn1 N1 84.1(3) C12 Mn1 N2 97.4(4) C12 Mn1 N1 175.1(4) C12 Mn1 C11 89.9(4) C12 Mn1 N3 92.1(4) C13 Mn1 N2 173.5(4) C13 Mn1 N1 95.2(4) C13 Mn1 C11 88.8(4) C13 Mn1 N3 96.5(4) C13 Mn1 C12 88.3(4) Mo3 O10 Mo5 151.3(3) Mo2 O15 Mo11 151.0(3) Mo9 O26 Mo10 152.3(3) Mo10 O30 Mo1 151.2(2) Mo6 O3 Mo8 151.1(3) Mo2 O33 Mo1 126.8(2) C44 N9 Mn3 171.0(7) Mo4 O9 Mo5 126.3(2) Mo8 O21 Mo7 152.2(3) Mo1 O34 Mo9 150.3(3) Mo7 O24 Mo12 126.0(2) Mo12 O38 Mo3 150.9(3) Mo5 O8 Mo12 151.7(3) Mo4 O12 Mo2 151.3(3) Mo8 O19 Mo10 124.8(2) Mo1 O32 Mo3 125.7(3) Mo11 O13 Mo4 151.3(3) Mo5 O4 Mo6 126.5(2) Mo6 O5 Mo4 126.9(3) Mo7 O2 Mo6 151.6(3) Mo9 O23 Mo7 125.2(2) C6 N2 Mn1 115.3(5) C10 N2 Mn1 126.2(5) C10 N2 C6 118.3(7) C40 N8 Mn3 126.4(6) C40 N8 C36 118.3(7) C36 N8 Mn3 114.7(5) O45 C27 Mn2 177.5(8) Mo12 O27 Mo9 125.2(3) Mo11 O16 Mo8 126.1(2) Mo3 O37 Mo2 125.5(2) C20 N4 Mn2 115.7(5) C16 N4 Mn2 126.2(5) C16 N4 C20 118.1(7) C5 N1 Mn1 115.1(5) C1 N1 Mn1 127.3(6) C1 N1 C5 117.6(7) Mo10 O17 Mo11 125.2(2) Mo12 O28 Mo9 89.24(15) Mo12 O28 Mo7 89.56(14) Mo7 O28 Mo9 89.12(14) P1 O28 Mo9 126.4(2) P1 O28 Mo12 125.9(2) P1 O28 Mo7 124.9(2) C25 N5 Mn2 126.5(6) C25 N5 C21 118.5(7) C21 N5 Mn2 114.8(5) C35 N7 Mn3 115.2(5) C31 N7 Mn3 125.6(6) C31 N7 C35 118.7(8) C29 N6 Mn2 174.6(7) N2 C6 C5 114.5(7) N2 C6 C7 120.7(7) C7 C6 C5 124.8(7) N1 C5 C6 115.2(6) N1 C5 C4 121.4(7) C4 C5 C6 123.4(7) C6 C7 H7 120.1 C6 C7 C8 119.7(8) C8 C7 H7 120.1 C5 C4 H4 120.1 C3 C4 C5 119.8(8) C3 C4 H4 120.1 Mo1 O35 Mo2 89.33(14) Mo3 O35 Mo1 89.21(15) Mo3 O35 Mo2 89.38(14) P1 O35 Mo1 125.7(2) P1 O35 Mo3 125.9(2) P1 O35 Mo2 125.6(2) O41 C11 Mn1 178.2(8) N4 C20 C19 120.8(7) N4 C20 C21 114.8(7) C19 C20 C21 124.3(7) N7 C35 C36 115.3(8) N7 C35 C34 120.9(8) C34 C35 C36 123.8(8) N2 C10 H10 118.4 N2 C10 C9 123.1(8) C9 C10 H10 118.4 C16 C17 H17 121.3 C18 C17 H17 121.3 C18 C17 C16 117.3(8) C39 C38 H38 120.5 C39 C38 C37 118.9(9) C37 C38 H38 120.5 C14 N3 Mn1 173.2(8) N8 C40 H40 118.7 N8 C40 C39 122.7(8) C39 C40 H40 118.7 N9 C44 C45 176.9(10) O46 C28 Mn2 178.6(8) C4 C3 H3 120.7 C2 C3 C4 118.5(8) C2 C3 H3 120.7 N8 C36 C35 114.3(8) N8 C36 C37 121.1(8) C37 C36 C35 124.6(8) C3 C2 H2 120.0 C3 C2 C1 120.0(8) C1 C2 H2 120.0 N6 C29 C30 178.1(9) C38 C39 C40 118.5(8) C38 C39 H39 120.7 C40 C39 H39 120.7 C20 C19 H19 120.4 C18 C19 C20 119.2(8) C18 C19 H19 120.4 C33 C32 H32 120.7 C33 C32 C31 118.5(9) C31 C32 H32 120.7 N4 C16 C17 124.0(7) N4 C16 H16 118.0 C17 C16 H16 118.0 C29 C30 H30A 109.5 C29 C30 H30B 109.5 C29 C30 H30C 109.5 H30A C30 H30B 109.5 H30A C30 H30C 109.5 H30B C30 H30C 109.5 Mo10 O18 Mo8 88.91(14) Mo10 O18 Mo11 89.54(14) Mo8 O18 Mo11 88.98(15) P1 O18 Mo10 125.8(2) P1 O18 Mo8 125.7(2) P1 O18 Mo11 126.1(2) C44 C45 H45A 109.5 C44 C45 H45B 109.5 C44 C45 H45C 109.5 H45A C45 H45B 109.5 H45A C45 H45C 109.5 H45B C45 H45C 109.5 C38 C37 C36 120.4(9) C38 C37 H37 119.8 C36 C37 H37 119.8 N5 C25 H25 118.9 N5 C25 C24 122.1(8) C24 C25 H25 118.9 C17 C18 H18 119.7 C19 C18 C17 120.6(8) C19 C18 H18 119.7 N1 C1 C2 122.7(8) N1 C1 H1 118.7 C2 C1 H1 118.7 N5 C21 C20 115.3(6) N5 C21 C22 121.2(7) C22 C21 C20 123.5(8) O49 C43 Mn3 179.6(10) C32 C33 H33 119.8 C32 C33 C34 120.4(9) C34 C33 H33 119.8 Mo5 O6 Mo6 89.51(14) Mo5 O6 Mo4 89.05(14) Mo6 O6 Mo4 89.18(15) P1 O6 Mo5 125.9(3) P1 O6 Mo6 126.2(2) P1 O6 Mo4 125.3(2) C7 C8 H8 120.0 C9 C8 C7 120.0(8) C9 C8 H8 120.0 C10 C9 H9 121.0 C8 C9 C10 118.0(8) C8 C9 H9 121.0 N7 C31 C32 123.0(9) N7 C31 H31 118.5 C32 C31 H31 118.5 O42 C12 Mn1 178.6(9) C35 C34 H34 120.8 C33 C34 C35 118.5(9) C33 C34 H34 120.8 N3 C14 C15 177.5(11) C21 C22 H22 120.3 C23 C22 C21 119.3(8) C23 C22 H22 120.3 C22 C23 H23 120.3 C24 C23 C22 119.4(8) C24 C23 H23 120.3 C25 C24 H24 120.4 C23 C24 C25 119.3(8) C23 C24 H24 120.4 C14 C15 H15A 109.5 C14 C15 H15B 109.5 C14 C15 H15C 109.5 H15A C15 H15B 109.5 H15A C15 H15C 109.5 H15B C15 H15C 109.5 O44 C26 Mn2 178.6(8) O43 C13 Mn1 173.0(10) N10 C46 C47 171.7(14) C46 C47 H47A 109.5 C46 C47 H47B 109.5 C46 C47 H47C 109.5 H47A C47 H47B 109.5 H47A C47 H47C 109.5 H47B C47 H47C 109.5 H49A C49 H49B 109.5 H49A C49 H49C 109.5 H49B C49 H49C 109.5 C48 C49 H49A 109.5 C48 C49 H49B 109.5 C48 C49 H49C 109.5 N11 C48 C49 176.4(13) O47 C41 Mn3 176.9(9) O48 C42 Mn3 177.4(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Mo1 O30 1.956(4) Mo1 O33 1.984(5) Mo1 O34 1.843(5) Mo1 O32 1.870(5) Mo1 O31 1.664(5) Mo1 O35 2.439(4) Mo10 O26 1.968(5) Mo10 O30 1.850(4) Mo10 O29 1.670(5) Mo10 O19 1.960(5) Mo10 O17 1.883(5) Mo10 O18 2.428(4) Mo8 O3 1.975(5) Mo8 O21 1.848(5) Mo8 O19 1.880(5) Mo8 O20 1.666(5) Mo8 O16 1.959(5) Mo8 O18 2.431(4) Mo9 O26 1.841(4) Mo9 O34 1.982(5) Mo9 O23 1.848(5) Mo9 O27 1.982(5) Mo9 O28 2.443(4) Mo9 O25 1.674(5) Mo3 O10 1.854(5) Mo3 O38 1.974(5) Mo3 O32 1.968(5) Mo3 O37 1.857(5) Mo3 O36 1.676(5) Mo3 O35 2.424(4) Mo5 O10 1.967(5) Mo5 O9 1.981(5) Mo5 O8 1.858(5) Mo5 O4 1.860(5) Mo5 O7 1.677(5) Mo5 O6 2.433(4) Mo6 O3 1.847(4) Mo6 O4 1.988(5) Mo6 O5 1.855(5) Mo6 O2 1.966(5) Mo6 O1 1.665(5) Mo6 O6 2.448(4) Mo2 O15 1.843(5) Mo2 O33 1.859(5) Mo2 O12 1.971(5) Mo2 O40 1.666(5) Mo2 O37 1.998(5) Mo2 O35 2.450(4) Mo11 O15 1.970(5) Mo11 O13 1.838(5) Mo11 O16 1.878(5) Mo11 O17 1.985(5) Mo11 O14 1.669(5) Mo11 O18 2.450(4) Mo12 O24 1.969(5) Mo12 O38 1.852(5) Mo12 O8 1.973(5) Mo12 O27 1.869(5) Mo12 O28 2.425(4) Mo12 O39 1.678(5) Mo7 O21 1.957(5) Mo7 O24 1.872(5) Mo7 O2 1.847(5) Mo7 O23 2.007(5) Mo7 O22 1.663(5) Mo7 O28 2.435(4) Mo4 O9 1.859(5) Mo4 O12 1.845(5) Mo4 O13 1.973(5) Mo4 O5 1.991(5) Mo4 O11 1.666(5) Mo4 O6 2.454(4) P1 O28 1.536(5) P1 O35 1.530(5) P1 O18 1.537(4) P1 O6 1.524(4) Mn2 C27 1.815(9) Mn2 N4 2.044(6) Mn2 N5 2.056(6) Mn2 N6 2.029(7) Mn2 C28 1.790(9) Mn2 C26 1.815(8) Mn3 N9 2.011(7) Mn3 N8 2.052(7) Mn3 N7 2.034(7) Mn3 C43 1.788(9) Mn3 C41 1.805(9) Mn3 C42 1.805(9) Mn1 N2 2.030(6) Mn1 N1 2.037(6) Mn1 C11 1.794(9) Mn1 N3 2.012(7) Mn1 C12 1.787(9) Mn1 C13 1.784(10) N9 C44 1.121(10) N2 C6 1.361(9) N2 C10 1.331(9) N8 C40 1.334(9) N8 C36 1.350(10) C27 O45 1.130(9) N4 C20 1.354(9) N4 C16 1.343(9) N1 C5 1.354(9) N1 C1 1.344(10) N5 C25 1.341(10) N5 C21 1.354(10) N7 C35 1.339(10) N7 C31 1.329(10) N6 C29 1.120(9) C6 C5 1.454(10) C6 C7 1.368(10) C5 C4 1.387(10) C7 H7 0.9300 C7 C8 1.377(11) C4 H4 0.9300 C4 C3 1.378(11) C11 O41 1.148(9) C20 C19 1.392(11) C20 C21 1.455(10) C35 C36 1.467(11) C35 C34 1.404(12) C10 H10 0.9300 C10 C9 1.381(11) C17 H17 0.9300 C17 C16 1.372(11) C17 C18 1.371(11) C38 H38 0.9300 C38 C39 1.366(12) C38 C37 1.368(11) N3 C14 1.120(10) C40 H40 0.9300 C40 C39 1.391(12) C44 C45 1.466(12) C28 O46 1.146(10) C3 H3 0.9300 C3 C2 1.355(11) C36 C37 1.375(12) C2 H2 0.9300 C2 C1 1.373(11) C29 C30 1.459(11) C39 H39 0.9300 C19 H19 0.9300 C19 C18 1.371(11) C32 H32 0.9300 C32 C33 1.339(12) C32 C31 1.385(12) C16 H16 0.9300 C30 H30A 0.9600 C30 H30B 0.9600 C30 H30C 0.9600 C45 H45A 0.9600 C45 H45B 0.9600 C45 H45C 0.9600 C37 H37 0.9300 C25 H25 0.9300 C25 C24 1.381(11) C18 H18 0.9300 C1 H1 0.9300 C21 C22 1.388(10) C43 O49 1.166(10) C33 H33 0.9300 C33 C34 1.378(12) C8 H8 0.9300 C8 C9 1.356(11) C9 H9 0.9300 C31 H31 0.9300 O42 C12 1.166(10) C34 H34 0.9300 C14 C15 1.454(12) C22 H22 0.9300 C22 C23 1.373(11) C23 H23 0.9300 C23 C24 1.362(12) C24 H24 0.9300 O44 C26 1.143(9) C15 H15A 0.9600 C15 H15B 0.9600 C15 H15C 0.9600 O43 C13 1.156(11) N11 C48 1.136(13) C46 C47 1.383(9) C46 N10 1.139(8) C47 H47A 0.9600 C47 H47B 0.9600 C47 H47C 0.9600 C49 H49A 0.9600 C49 H49B 0.9600 C49 H49C 0.9600 C49 C48 1.409(14) O47 C41 1.147(10) O48 C42 1.143(10) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C7 H7 O29 0.93 2.45 3.133(9) 130.3 1_565 yes C10 H10 O4 0.93 2.45 3.186(9) 136.1 . yes C19 H19 O7 0.93 2.63 3.334(10) 133.1 2_666 yes C32 H32 O36 0.93 2.53 3.274(10) 137.3 2_665 yes C16 H16 O30 0.93 2.54 3.232(9) 131.1 2_656 yes C30 H30B O24 0.96 2.61 3.135(9) 114.6 2_666 yes C45 H45B N11 0.96 2.64 3.437(15) 140.9 2_666 yes C45 H45C O9 0.96 2.63 3.523(10) 154.6 1_455 yes C45 H45C O12 0.96 2.65 3.460(10) 141.8 1_455 yes C31 H31 O7 0.93 2.63 3.445(11) 146.5 2_665 yes C47 H47A O45 0.96 2.55 3.513(15) 178.3 1_554 yes C47 H47C O33 0.96 2.48 3.111(14) 123.1 . yes