#------------------------------------------------------------------------------ #$Date: 2020-08-28 04:44:41 +0300 (Fri, 28 Aug 2020) $ #$Revision: 255703 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705289.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_7705289 loop_ _publ_author_name 'Qu, Di' 'Liu, Xiaoting' 'Duan, Fengxue' 'xue, rong' 'Li, Bao' 'Wu, Lixin' _publ_section_title ; {VMo9O31[RC(CH2O)3]}6−: the first class of triol ligand covalently-decorated Keggin-type polyoxomolybdates ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT02506B _journal_year 2020 _chemical_formula_moiety 'C5 H9 Mo9 O35 V, 9(H2 O), 6(N H4)' _chemical_formula_sum 'C5 H51 Mo9 N6 O44 V' _chemical_formula_weight 1813.92 _space_group_crystal_system orthorhombic _space_group_IT_number 36 _space_group_name_Hall 'C 2c -2' _space_group_name_H-M_alt 'C m c 21' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2020-08-06 deposited with the CCDC. 2020-08-27 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.8761(9) _cell_length_b 16.0198(10) _cell_length_c 20.6578(13) _cell_measurement_reflns_used 9842 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.50 _cell_measurement_theta_min 2.73 _cell_volume 4592.1(5) _computing_cell_refinement 'Bruker D8 Venture' _computing_data_collection 'Bruker D8 Venture' _computing_data_reduction 'Bruker D8 Venture' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'D8 VENTURE PHOTON II' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_unetI/netI 0.0307 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 23232 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.531 _diffrn_reflns_theta_min 2.727 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 2.686 _exptl_absorpt_correction_T_max 0.775 _exptl_absorpt_correction_T_min 0.722 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS; Bruker, 2014' _exptl_crystal_colour yellow-green _exptl_crystal_density_diffrn 2.624 _exptl_crystal_description block _exptl_crystal_F_000 3504 _exptl_crystal_size_max 0.130 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.100 _refine_diff_density_max 1.028 _refine_diff_density_min -0.891 _refine_diff_density_rms 0.122 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.47(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 324 _refine_ls_number_reflns 5282 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.075 _refine_ls_R_factor_all 0.0278 _refine_ls_R_factor_gt 0.0260 _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^)+(0.0377P)^2^+10.1667P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0677 _refine_ls_wR_factor_ref 0.0693 _reflns_Friedel_coverage 0.946 _reflns_Friedel_fraction_full 0.998 _reflns_Friedel_fraction_max 0.997 _reflns_number_gt 5075 _reflns_number_total 5282 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02506b2.cif _cod_data_source_block mo_LXT0711_10_0m _cod_database_code 7705289 _shelx_shelxl_version_number 2014/7 _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_min 0.722 _shelx_estimated_absorpt_t_max 0.775 _shelx_res_file ; mo_LXT0711_10_0m.res created by SHELXL-2014/7 TITL mo_LXT0711_10_0m_a.res in Cmc2(1) CELL 0.71073 13.8761 16.0198 20.6578 90 90 90 ZERR 4 0.0009 0.001 0.0013 0 0 0 LATT -7 SYMM -X,-Y,0.5+Z SYMM -X,+Y,+Z SYMM +X,-Y,0.5+Z SFAC C H N O V Mo UNIT 20 204 24 176 4 36 L.S. 8 PLAN -10 SIZE 0.1 0.12 0.13 BOND $H fmap 2 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 REM REM REM omit 1 3 -2 omit 1 3 2 WGHT 0.037700 10.166700 BASF 0.47431 FVAR 0.10355 N3 3 0.500000 0.614293 0.808693 10.50000 0.05092 0.04379 = 0.03900 -0.00184 0.00000 0.00000 AFIX 3 H3A 2 0.500000 0.565623 0.787923 10.50000 -1.20000 H3B 2 0.552370 0.617884 0.833403 10.50000 -1.20000 H3C 2 0.447630 0.617884 0.833403 10.50000 -1.20000 AFIX 3 H3D 2 0.500000 0.656703 0.779393 10.50000 -1.20000 AFIX 0 C1 1 0.590350 0.332262 0.634627 11.00000 0.03422 0.02124 = 0.02933 0.00260 -0.00083 0.00436 AFIX 23 H1A 2 0.646607 0.327094 0.662210 11.00000 -1.20000 H1B 2 0.589768 0.284914 0.605361 11.00000 -1.20000 AFIX 0 C2 1 0.500000 0.401212 0.725873 10.50000 0.03242 0.02460 = 0.02539 0.00490 0.00000 0.00000 AFIX 23 H2A 2 0.443511 0.396208 0.753259 10.50000 -1.20000 H2B 2 0.556489 0.396208 0.753259 10.50000 -1.20000 AFIX 0 C3 1 0.500000 0.329801 0.676484 10.50000 0.03683 0.02254 = 0.01975 0.00269 0.00000 0.00000 PART -1 C4 1 0.496224 0.246571 0.713296 10.50000 0.06646 0.03399 = 0.04359 0.01532 0.00575 0.03114 AFIX 23 H4A 2 0.497521 0.202435 0.681162 10.50000 -1.20000 H4B 2 0.555603 0.242140 0.737836 10.50000 -1.20000 AFIX 0 O21 4 0.426371 0.229883 0.752627 10.50000 0.08209 0.06170 = 0.06420 0.01966 0.01482 -0.01280 AFIX 147 H21 2 0.432419 0.257801 0.785649 10.50000 -1.50000 AFIX 0 PART 0 MO1 6 0.621088 0.759573 0.661554 11.00000 0.03386 0.02439 = 0.02173 -0.00354 -0.00046 -0.00553 MO2 6 0.758208 0.656392 0.524157 11.00000 0.03034 0.03097 = 0.02549 -0.00188 0.00598 -0.00769 MO3 6 0.636657 0.568097 0.401003 11.00000 0.03918 0.03235 = 0.01809 -0.00233 0.00589 -0.00288 MO4 6 0.500000 0.426713 0.517485 10.50000 0.02761 0.02147 = 0.01728 -0.00160 0.00000 0.00000 MO5 6 0.628433 0.522515 0.647719 11.00000 0.02328 0.02279 = 0.01856 -0.00012 -0.00070 -0.00093 N1 3 0.714727 0.904131 0.511164 11.00000 0.05643 0.04839 = 0.04782 0.00216 0.00834 -0.00673 AFIX 3 H1C 2 0.728417 0.900851 0.469155 11.00000 -1.20000 H1D 2 0.752558 0.942121 0.529674 11.00000 -1.20000 H1E 2 0.724588 0.854691 0.529674 11.00000 -1.20000 H1F 2 0.651958 0.919201 0.516284 11.00000 -1.20000 AFIX 0 N2 3 0.500000 0.166792 0.435577 10.50000 0.08093 0.06037 = 0.07559 -0.00868 0.00000 0.00000 AFIX 3 H2C 2 0.500000 0.174652 0.392937 10.50000 -1.20000 H2D 2 0.552370 0.138242 0.446927 10.50000 -1.20000 H2E 2 0.447630 0.138242 0.446927 10.50000 -1.20000 H2F 2 0.500000 0.217122 0.455997 10.50000 -1.20000 AFIX 0 O26 4 0.603143 0.827762 0.397738 11.00000 0.10166 0.06061 = 0.08085 0.00181 -0.01579 -0.00032 AFIX 3 H26A 2 0.604204 0.776661 0.386656 11.00000 -1.50000 H26B 2 0.605602 0.833342 0.438688 11.00000 -1.50000 AFIX 0 O1 4 0.500000 0.760066 0.707873 10.50000 0.03743 0.02523 = 0.02056 -0.00448 0.00000 0.00000 O2 4 0.699640 0.765859 0.725762 11.00000 0.04039 0.04175 = 0.03167 -0.00862 -0.00335 -0.01064 O3 4 0.616446 0.860054 0.632845 11.00000 0.05608 0.02944 = 0.03796 -0.00121 0.00475 -0.00542 O4 4 0.701303 0.716178 0.594313 11.00000 0.03719 0.02970 = 0.02688 -0.00716 0.00491 -0.00753 O5 4 0.500000 0.724181 0.590101 10.50000 0.03469 0.02308 = 0.02216 -0.00393 0.00000 0.00000 O6 4 0.608967 0.623162 0.681014 11.00000 0.02958 0.02502 = 0.02743 -0.00192 0.00250 -0.00390 O7 4 0.872229 0.635119 0.551711 11.00000 0.03622 0.04852 = 0.04852 -0.00576 0.00314 -0.00636 O8 4 0.775612 0.741192 0.474818 11.00000 0.05451 0.03719 = 0.03521 -0.00011 0.01067 -0.01347 O9 4 0.750370 0.573216 0.456376 11.00000 0.03507 0.03418 = 0.02740 -0.00323 0.00649 -0.00066 O10 4 0.600077 0.649523 0.489131 11.00000 0.03706 0.02576 = 0.01888 -0.00076 0.00154 -0.00380 O11 4 0.705370 0.551309 0.582912 11.00000 0.03100 0.02742 = 0.02444 -0.00137 0.00398 -0.00187 O12 4 0.657074 0.657870 0.358655 11.00000 0.06155 0.04071 = 0.03243 0.00572 0.00644 -0.00897 O13 4 0.673274 0.491295 0.349764 11.00000 0.04999 0.04562 = 0.03147 -0.01180 0.00941 0.00095 O14 4 0.500000 0.562855 0.390332 10.50000 0.04458 0.03669 = 0.02000 0.00421 0.00000 0.00000 O15 4 0.402230 0.470393 0.473165 11.00000 0.03520 0.02746 = 0.02139 -0.00158 -0.00344 -0.00045 O16 4 0.500000 0.324312 0.497983 10.50000 0.04372 0.02984 = 0.03447 -0.00410 0.00000 0.00000 O17 4 0.598004 0.408729 0.597055 11.00000 0.02696 0.02421 = 0.01948 -0.00018 0.00007 0.00036 O18 4 0.500000 0.547946 0.579391 10.50000 0.02703 0.02667 = 0.01454 0.00039 0.00000 0.00000 O19 4 0.500000 0.482219 0.695777 10.50000 0.02616 0.01986 = 0.01832 0.00121 0.00000 0.00000 O20 4 0.701372 0.472752 0.701864 11.00000 0.02973 0.03242 = 0.03066 0.00187 -0.00619 0.00269 O22 4 0.500000 0.954669 0.528921 10.50000 0.07284 0.30645 = 0.19279 0.11438 0.00000 0.00000 AFIX 3 H22A 2 0.500000 0.931396 0.565774 10.50000 -1.50000 H22B 2 0.455013 0.919272 0.506729 10.50000 -1.50000 AFIX 0 O23 4 0.861405 0.767739 0.355087 11.00000 0.09348 0.14554 = 0.04196 -0.00166 0.01517 -0.04923 AFIX 3 H23A 2 0.845770 0.789824 0.390991 11.00000 -1.50000 H23B 2 0.810393 0.743554 0.342186 11.00000 -1.50000 AFIX 0 O24 4 0.597708 0.035291 0.667851 11.00000 0.06141 0.06548 = 0.08735 0.00723 0.01995 0.00524 AFIX 3 H24A 2 0.606762 0.064378 0.633977 11.00000 -1.50000 H24B 2 0.603262 -0.015922 0.657877 11.00000 -1.50000 AFIX 0 O25 4 0.618682 0.924562 0.796507 11.00000 0.43982 0.18590 = 0.13631 -0.03228 0.04138 -0.04216 AFIX 3 H25A 2 0.587788 0.936936 0.762295 11.00000 -1.50000 H25B 2 0.618200 0.871522 0.797563 11.00000 -1.50000 AFIX 0 N4 3 0.801322 0.383920 0.279048 11.00000 0.05296 0.05946 = 0.05670 -0.00045 0.01049 0.01065 AFIX 3 H4C 2 0.792738 0.391211 0.236725 11.00000 -1.20000 H4D 2 0.862015 0.396025 0.289361 11.00000 -1.20000 H4E 2 0.788904 0.331043 0.289312 11.00000 -1.20000 H4F 2 0.760756 0.418138 0.301260 11.00000 -1.20000 AFIX 0 V1 5 0.500000 0.645194 0.535945 10.50000 0.02878 0.02069 = 0.01467 0.00033 0.00000 0.00000 HKLF 4 REM mo_LXT0711_10_0m_a.res in Cmc2(1) REM R1 = 0.0260 for 5075 Fo > 4sig(Fo) and 0.0278 for all 5282 data REM 324 parameters refined using 1 restraints END WGHT 0.0385 7.5545 REM Highest difference peak 1.028, deepest hole -0.891, 1-sigma level 0.122 Q1 1 0.0778 0.5123 0.4049 11.00000 0.05 1.03 Q2 1 0.0000 0.5116 0.3963 10.50000 0.05 0.75 Q3 1 0.5000 0.1784 0.6956 10.50000 0.05 0.52 Q4 1 0.5000 0.9244 0.7702 10.50000 0.05 0.51 Q5 1 0.5000 0.4289 0.4505 10.50000 0.05 0.46 Q6 1 0.6277 0.8419 0.6679 11.00000 0.05 0.46 Q7 1 0.5509 0.3368 0.6631 11.00000 0.05 0.43 Q8 1 0.5000 0.2970 0.6924 10.50000 0.05 0.43 Q9 1 0.4676 0.5085 0.6447 11.00000 0.05 0.43 Q10 1 0.6227 0.9428 0.6610 11.00000 0.05 0.43 ; _shelx_res_checksum 68392 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' 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 N3 N 0.5000 0.6143(6) 0.8087(5) 0.045(2) Uani 1 2 d S T P . . H3A H 0.5000 0.5656 0.7879 0.053 Uiso 1 2 d R U P . . H3B H 0.5524 0.6179 0.8334 0.053 Uiso 0.5 1 d R U P . . H3C H 0.4476 0.6179 0.8334 0.053 Uiso 0.5 1 d R U P . . H3D H 0.5000 0.6567 0.7794 0.053 Uiso 1 2 d R U P . . C1 C 0.5903(5) 0.3323(4) 0.6346(3) 0.0283(13) Uani 1 1 d . . . . . H1A H 0.6466 0.3271 0.6622 0.034 Uiso 1 1 calc R U . . . H1B H 0.5898 0.2849 0.6054 0.034 Uiso 1 1 calc R U . . . C2 C 0.5000 0.4012(6) 0.7259(5) 0.0275(18) Uani 1 2 d S T P A . H2A H 0.4435 0.3962 0.7533 0.033 Uiso 0.5 1 calc R U P . . H2B H 0.5565 0.3962 0.7533 0.033 Uiso 0.5 1 calc R U P . . C3 C 0.5000 0.3298(5) 0.6765(4) 0.0264(17) Uani 1 2 d S T P . . C4 C 0.496(4) 0.2466(9) 0.7133(7) 0.048(5) Uani 0.5 1 d . . P A -1 H4A H 0.4975 0.2024 0.6812 0.058 Uiso 0.5 1 calc R U P A -1 H4B H 0.5556 0.2421 0.7378 0.058 Uiso 0.5 1 calc R U P A -1 O21 O 0.4264(12) 0.2299(9) 0.7526(8) 0.069(4) Uani 0.5 1 d . . P A -1 H21 H 0.4324 0.2578 0.7856 0.104 Uiso 0.5 1 calc R U P A -1 Mo1 Mo 0.62109(4) 0.75957(3) 0.66155(3) 0.02666(13) Uani 1 1 d . . . . . Mo2 Mo 0.75821(4) 0.65639(3) 0.52416(3) 0.02894(13) Uani 1 1 d . . . . . Mo3 Mo 0.63666(4) 0.56810(4) 0.40100(3) 0.02987(14) Uani 1 1 d . . . . . Mo4 Mo 0.5000 0.42671(4) 0.51749(4) 0.02212(16) Uani 1 2 d S T P . . Mo5 Mo 0.62843(3) 0.52251(3) 0.64772(2) 0.02155(12) Uani 1 1 d . . . . . N1 N 0.7147(6) 0.9041(4) 0.5112(4) 0.0509(18) Uani 1 1 d . . . . . H1C H 0.7284 0.9009 0.4692 0.061 Uiso 1 1 d R U . . . H1D H 0.7526 0.9421 0.5297 0.061 Uiso 1 1 d R U . . . H1E H 0.7246 0.8547 0.5297 0.061 Uiso 1 1 d R U . . . H1F H 0.6520 0.9192 0.5163 0.061 Uiso 1 1 d R U . . . N2 N 0.5000 0.1668(8) 0.4356(8) 0.072(4) Uani 1 2 d S T P . . H2C H 0.5000 0.1747 0.3929 0.087 Uiso 1 2 d R U P . . H2D H 0.5524 0.1382 0.4469 0.087 Uiso 0.5 1 d R U P . . H2E H 0.4476 0.1382 0.4469 0.087 Uiso 0.5 1 d R U P . . H2F H 0.5000 0.2171 0.4560 0.087 Uiso 1 2 d R U P . . O26 O 0.6031(7) 0.8278(5) 0.3977(5) 0.081(2) Uani 1 1 d . . . . . H26A H 0.6042 0.7767 0.3867 0.122 Uiso 1 1 d R U . . . H26B H 0.6056 0.8333 0.4387 0.122 Uiso 1 1 d R U . . . O1 O 0.5000 0.7601(4) 0.7079(3) 0.0277(13) Uani 1 2 d S T P . . O2 O 0.6996(4) 0.7659(3) 0.7258(3) 0.0379(12) Uani 1 1 d . . . . . O3 O 0.6164(4) 0.8601(3) 0.6328(3) 0.0412(13) Uani 1 1 d . . . . . O4 O 0.7013(3) 0.7162(3) 0.5943(2) 0.0313(10) Uani 1 1 d . . . . . O5 O 0.5000 0.7242(4) 0.5901(3) 0.0266(13) Uani 1 2 d S T P . . O6 O 0.6090(3) 0.6232(3) 0.6810(2) 0.0273(10) Uani 1 1 d . . . . . O7 O 0.8722(4) 0.6351(4) 0.5517(3) 0.0444(14) Uani 1 1 d . . . . . O8 O 0.7756(4) 0.7412(3) 0.4748(3) 0.0423(13) Uani 1 1 d . . . . . O9 O 0.7504(4) 0.5732(3) 0.4564(2) 0.0322(11) Uani 1 1 d . . . . . O10 O 0.6001(3) 0.6495(3) 0.4891(2) 0.0272(9) Uani 1 1 d . . . . . O11 O 0.7054(3) 0.5513(3) 0.5829(2) 0.0276(9) Uani 1 1 d . . . . . O12 O 0.6571(5) 0.6579(3) 0.3587(3) 0.0449(13) Uani 1 1 d . . . . . O13 O 0.6733(4) 0.4913(4) 0.3498(3) 0.0424(12) Uani 1 1 d . . . . . O14 O 0.5000 0.5629(4) 0.3903(3) 0.0338(15) Uani 1 2 d S T P . . O15 O 0.4022(3) 0.4704(3) 0.4732(2) 0.0280(9) Uani 1 1 d . . . . . O16 O 0.5000 0.3243(4) 0.4980(4) 0.0360(16) Uani 1 2 d S T P . . O17 O 0.5980(3) 0.4087(3) 0.5971(2) 0.0235(8) Uani 1 1 d . . . . . O18 O 0.5000 0.5479(4) 0.5794(3) 0.0227(12) Uani 1 2 d S T P . . O19 O 0.5000 0.4822(3) 0.6958(3) 0.0214(12) Uani 1 2 d S T P . . O20 O 0.7014(3) 0.4728(3) 0.7019(2) 0.0309(10) Uani 1 1 d . . . . . O22 O 0.5000 0.9547(16) 0.5289(13) 0.191(11) Uani 1 2 d S T P . . H22A H 0.5000 0.9314 0.5658 0.286 Uiso 1 2 d R U P . . H22B H 0.4550 0.9193 0.5067 0.286 Uiso 0.5 1 d R U P . . O23 O 0.8614(6) 0.7677(7) 0.3551(4) 0.094(3) Uani 1 1 d . . . . . H23A H 0.8458 0.7898 0.3910 0.140 Uiso 1 1 d R U . . . H23B H 0.8104 0.7436 0.3422 0.140 Uiso 1 1 d R U . . . O24 O 0.5977(5) 0.0353(5) 0.6679(5) 0.071(2) Uani 1 1 d . . . . . H24A H 0.6068 0.0644 0.6340 0.107 Uiso 1 1 d R U . . . H24B H 0.6033 -0.0159 0.6579 0.107 Uiso 1 1 d R U . . . O25 O 0.6187(17) 0.9246(12) 0.7965(9) 0.254(12) Uani 1 1 d . . . . . H25A H 0.5878 0.9369 0.7623 0.381 Uiso 1 1 d R U . . . H25B H 0.6182 0.8715 0.7976 0.381 Uiso 1 1 d R U . . . N4 N 0.8013(6) 0.3839(5) 0.2790(4) 0.0564(19) Uani 1 1 d . . . . . H4C H 0.7927 0.3912 0.2367 0.068 Uiso 1 1 d R U . . . H4D H 0.8620 0.3960 0.2894 0.068 Uiso 1 1 d R U . . . H4E H 0.7889 0.3310 0.2893 0.068 Uiso 1 1 d R U . . . H4F H 0.7608 0.4181 0.3013 0.068 Uiso 1 1 d R U . . . V1 V 0.5000 0.64519(8) 0.53594(7) 0.0214(3) Uani 1 2 d S T P . . 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 N3 0.051(6) 0.044(5) 0.039(5) -0.002(4) 0.000 0.000 C1 0.034(3) 0.021(3) 0.029(4) 0.003(3) -0.001(3) 0.004(2) C2 0.032(5) 0.025(4) 0.025(5) 0.005(4) 0.000 0.000 C3 0.037(5) 0.023(4) 0.020(4) 0.003(3) 0.000 0.000 C4 0.066(12) 0.034(7) 0.044(7) 0.015(6) 0.01(2) 0.031(17) O21 0.082(10) 0.062(10) 0.064(10) 0.020(7) 0.015(8) -0.013(7) Mo1 0.0339(3) 0.0244(3) 0.0217(3) -0.0035(2) -0.0005(2) -0.0055(2) Mo2 0.0303(3) 0.0310(3) 0.0255(3) -0.0019(3) 0.0060(2) -0.0077(2) Mo3 0.0392(3) 0.0324(3) 0.0181(3) -0.0023(2) 0.0059(2) -0.0029(2) Mo4 0.0276(3) 0.0215(3) 0.0173(3) -0.0016(3) 0.000 0.000 Mo5 0.0233(2) 0.0228(2) 0.0186(3) -0.0001(2) -0.00070(19) -0.00093(17) N1 0.056(4) 0.048(4) 0.048(5) 0.002(4) 0.008(4) -0.007(3) N2 0.081(9) 0.060(7) 0.076(9) -0.009(7) 0.000 0.000 O26 0.102(6) 0.061(5) 0.081(6) 0.002(5) -0.016(5) 0.000(4) O1 0.037(3) 0.025(3) 0.021(3) -0.004(2) 0.000 0.000 O2 0.040(3) 0.042(3) 0.032(3) -0.009(2) -0.003(2) -0.011(2) O3 0.056(3) 0.029(3) 0.038(3) -0.001(2) 0.005(2) -0.005(2) O4 0.037(2) 0.030(2) 0.027(2) -0.0072(19) 0.0049(19) -0.008(2) O5 0.035(3) 0.023(3) 0.022(3) -0.004(3) 0.000 0.000 O6 0.030(2) 0.025(2) 0.027(3) -0.0019(19) 0.0025(19) -0.0039(18) O7 0.036(3) 0.049(3) 0.049(4) -0.006(3) 0.003(2) -0.006(2) O8 0.055(3) 0.037(3) 0.035(3) 0.000(2) 0.011(2) -0.013(2) O9 0.035(2) 0.034(3) 0.027(2) -0.003(2) 0.006(2) -0.0007(19) O10 0.037(2) 0.026(2) 0.019(2) -0.0008(17) 0.0015(18) -0.0038(18) O11 0.031(2) 0.027(2) 0.024(2) -0.0014(18) 0.0040(18) -0.0019(18) O12 0.062(4) 0.041(3) 0.032(3) 0.006(2) 0.006(3) -0.009(3) O13 0.050(3) 0.046(3) 0.031(3) -0.012(2) 0.009(2) 0.001(3) O14 0.045(4) 0.037(4) 0.020(3) 0.004(3) 0.000 0.000 O15 0.035(2) 0.027(2) 0.021(2) -0.0016(17) -0.0034(18) -0.0005(18) O16 0.044(4) 0.030(3) 0.034(4) -0.004(3) 0.000 0.000 O17 0.027(2) 0.024(2) 0.019(2) -0.0002(17) 0.0001(17) 0.0004(17) O18 0.027(3) 0.027(3) 0.015(3) 0.000(2) 0.000 0.000 O19 0.026(3) 0.020(3) 0.018(3) 0.001(2) 0.000 0.000 O20 0.030(2) 0.032(3) 0.031(3) 0.0019(19) -0.0062(19) 0.0027(18) O22 0.073(10) 0.31(3) 0.19(2) 0.11(2) 0.000 0.000 O23 0.093(6) 0.146(9) 0.042(5) -0.002(5) 0.015(4) -0.049(6) O24 0.061(4) 0.065(4) 0.087(6) 0.007(4) 0.020(4) 0.005(3) O25 0.44(4) 0.186(18) 0.136(18) -0.032(15) 0.041(19) -0.042(17) N4 0.053(4) 0.059(5) 0.057(5) 0.000(4) 0.010(4) 0.011(4) V1 0.0288(7) 0.0207(7) 0.0147(7) 0.0003(5) 0.000 0.000 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' 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' V V 0.3005 0.5294 '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' 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 H3A N3 H3B 109.5 . . ? H3A N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? H3A N3 H3D 109.5 . . ? H3B N3 H3D 109.5 . . ? H3C N3 H3D 109.5 . . ? O17 C1 C3 112.6(5) . . ? O17 C1 H1A 109.1 . . ? C3 C1 H1A 109.1 . . ? O17 C1 H1B 109.1 . . ? C3 C1 H1B 109.1 . . ? H1A C1 H1B 107.8 . . ? O19 C2 C3 112.7(7) . . ? O19 C2 H2A 109.1 . . ? C3 C2 H2A 109.1 . . ? O19 C2 H2B 109.1 . . ? C3 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? C1 C3 C1 110.8(8) . 3_655 ? C1 C3 C2 111.0(5) . . ? C1 C3 C2 111.0(5) 3_655 . ? C1 C3 C4 109.4(18) . . ? C1 C3 C4 106(2) 3_655 . ? C2 C3 C4 108.6(9) . . ? O21 C4 C3 121(3) . . ? O21 C4 H4A 107.1 . . ? C3 C4 H4A 107.1 . . ? O21 C4 H4B 107.1 . . ? C3 C4 H4B 107.1 . . ? H4A C4 H4B 106.8 . . ? C4 O21 H21 109.5 . . ? O3 Mo1 O2 103.6(3) . . ? O3 Mo1 O4 96.4(2) . . ? O2 Mo1 O4 102.3(2) . . ? O3 Mo1 O1 97.7(3) . . ? O2 Mo1 O1 99.7(2) . . ? O4 Mo1 O1 150.2(2) . . ? O3 Mo1 O6 168.3(2) . . ? O2 Mo1 O6 88.1(2) . . ? O4 Mo1 O6 79.53(19) . . ? O1 Mo1 O6 81.3(2) . . ? O3 Mo1 O5 89.0(3) . . ? O2 Mo1 O5 165.8(2) . . ? O4 Mo1 O5 82.52(18) . . ? O1 Mo1 O5 71.6(2) . . ? O6 Mo1 O5 79.6(2) . . ? O8 Mo2 O7 103.0(3) . . ? O8 Mo2 O4 96.4(2) . . ? O7 Mo2 O4 103.3(3) . . ? O8 Mo2 O9 97.1(2) . . ? O7 Mo2 O9 98.9(3) . . ? O4 Mo2 O9 150.6(2) . . ? O8 Mo2 O11 168.6(2) . . ? O7 Mo2 O11 88.4(2) . . ? O4 Mo2 O11 80.05(19) . . ? O9 Mo2 O11 81.59(18) . . ? O8 Mo2 O10 89.2(2) . . ? O7 Mo2 O10 165.7(2) . . ? O4 Mo2 O10 82.47(19) . . ? O9 Mo2 O10 71.80(19) . . ? O11 Mo2 O10 79.64(17) . . ? O13 Mo3 O12 103.9(3) . . ? O13 Mo3 O14 101.1(3) . . ? O12 Mo3 O14 98.2(3) . . ? O13 Mo3 O9 98.8(2) . . ? O12 Mo3 O9 97.5(3) . . ? O14 Mo3 O9 150.7(3) . . ? O13 Mo3 O15 88.9(2) . 3_655 ? O12 Mo3 O15 167.2(2) . 3_655 ? O14 Mo3 O15 78.8(2) . 3_655 ? O9 Mo3 O15 80.39(19) . 3_655 ? O13 Mo3 O10 166.0(2) . . ? O12 Mo3 O10 88.0(2) . . ? O14 Mo3 O10 84.1(2) . . ? O9 Mo3 O10 71.94(19) . . ? O15 Mo3 O10 79.34(16) 3_655 . ? O16 Mo4 O15 105.0(2) . . ? O16 Mo4 O15 105.0(2) . 3_655 ? O15 Mo4 O15 99.3(3) . 3_655 ? O16 Mo4 O17 93.0(2) . . ? O15 Mo4 O17 157.95(19) . . ? O15 Mo4 O17 87.9(2) 3_655 . ? O16 Mo4 O17 93.0(2) . 3_655 ? O15 Mo4 O17 87.9(2) . 3_655 ? O15 Mo4 O17 157.94(19) 3_655 3_655 ? O17 Mo4 O17 78.4(2) . 3_655 ? O16 Mo4 O18 160.4(3) . . ? O15 Mo4 O18 87.39(17) . . ? O15 Mo4 O18 87.40(17) 3_655 . ? O17 Mo4 O18 72.05(16) . . ? O17 Mo4 O18 72.05(16) 3_655 . ? O20 Mo5 O11 105.0(2) . . ? O20 Mo5 O6 105.1(2) . . ? O11 Mo5 O6 98.5(2) . . ? O20 Mo5 O19 92.8(2) . . ? O11 Mo5 O19 158.5(2) . . ? O6 Mo5 O19 88.1(2) . . ? O20 Mo5 O17 92.3(2) . . ? O11 Mo5 O17 88.35(19) . . ? O6 Mo5 O17 158.79(19) . . ? O19 Mo5 O17 78.8(2) . . ? O20 Mo5 O18 160.2(2) . . ? O11 Mo5 O18 87.55(19) . . ? O6 Mo5 O18 87.7(2) . . ? O19 Mo5 O18 72.19(18) . . ? O17 Mo5 O18 72.5(2) . . ? H1C N1 H1D 109.5 . . ? H1C N1 H1E 109.5 . . ? H1D N1 H1E 109.5 . . ? H1C N1 H1F 109.5 . . ? H1D N1 H1F 109.5 . . ? H1E N1 H1F 109.5 . . ? H2C N2 H2D 109.5 . . ? H2C N2 H2E 109.5 . . ? H2D N2 H2E 109.5 . . ? H2C N2 H2F 109.5 . . ? H2D N2 H2F 109.5 . . ? H2E N2 H2F 109.5 . . ? H26A O26 H26B 111.6 . . ? Mo1 O1 Mo1 120.7(3) 3_655 . ? Mo2 O4 Mo1 167.3(3) . . ? V1 O5 Mo1 127.43(18) . 3_655 ? V1 O5 Mo1 127.43(18) . . ? Mo1 O5 Mo1 93.5(2) 3_655 . ? Mo5 O6 Mo1 144.1(3) . . ? Mo2 O9 Mo3 119.9(2) . . ? V1 O10 Mo3 127.6(2) . . ? V1 O10 Mo2 127.0(2) . . ? Mo3 O10 Mo2 93.75(17) . . ? Mo5 O11 Mo2 144.7(3) . . ? Mo3 O14 Mo3 165.8(4) . 3_655 ? Mo4 O15 Mo3 143.6(3) . 3_655 ? C1 O17 Mo5 118.0(4) . . ? C1 O17 Mo4 118.3(4) . . ? Mo5 O17 Mo4 112.54(19) . . ? V1 O18 Mo5 117.3(2) . . ? V1 O18 Mo5 117.3(2) . 3_655 ? Mo5 O18 Mo5 101.0(2) . 3_655 ? V1 O18 Mo4 116.7(3) . . ? Mo5 O18 Mo4 100.9(2) . . ? Mo5 O18 Mo4 100.9(2) 3_655 . ? C2 O19 Mo5 118.2(2) . 3_655 ? C2 O19 Mo5 118.2(2) . . ? Mo5 O19 Mo5 112.8(3) 3_655 . ? H22A O22 H22B 99.7 . . ? H23A O23 H23B 104.5 . . ? H24A O24 H24B 108.4 . . ? H25A O25 H25B 104.5 . . ? H4C N4 H4D 109.5 . . ? H4C N4 H4E 109.4 . . ? H4D N4 H4E 109.5 . . ? H4C N4 H4F 109.5 . . ? H4D N4 H4F 109.5 . . ? H4E N4 H4F 109.5 . . ? O5 V1 O10 110.34(19) . . ? O5 V1 O10 110.34(19) . 3_655 ? O10 V1 O10 110.2(3) . 3_655 ? O5 V1 O18 108.6(3) . . ? O10 V1 O18 108.69(18) . . ? O10 V1 O18 108.69(19) 3_655 . ? 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 N3 H3A 0.8899 . ? N3 H3B 0.8899 . ? N3 H3C 0.8899 . ? N3 H3D 0.9099 . ? C1 O17 1.454(7) . ? C1 C3 1.523(8) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 O19 1.439(10) . ? C2 C3 1.533(13) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C1 1.524(8) 3_655 ? C3 C4 1.536(15) . ? C4 O21 1.29(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? O21 H21 0.8200 . ? Mo1 O3 1.717(5) . ? Mo1 O2 1.720(5) . ? Mo1 O4 1.911(5) . ? Mo1 O1 1.934(3) . ? Mo1 O6 2.228(5) . ? Mo1 O5 2.307(4) . ? Mo2 O8 1.715(5) . ? Mo2 O7 1.716(5) . ? Mo2 O4 1.908(5) . ? Mo2 O9 1.936(5) . ? Mo2 O11 2.201(5) . ? Mo2 O10 2.313(5) . ? Mo3 O13 1.701(5) . ? Mo3 O12 1.707(5) . ? Mo3 O14 1.9109(11) . ? Mo3 O9 1.951(5) . ? Mo3 O15 2.228(5) 3_655 ? Mo3 O10 2.296(5) . ? Mo4 O16 1.689(7) . ? Mo4 O15 1.780(5) . ? Mo4 O15 1.780(5) 3_655 ? Mo4 O17 2.153(4) . ? Mo4 O17 2.153(4) 3_655 ? Mo4 O18 2.325(6) . ? Mo5 O20 1.706(5) . ? Mo5 O11 1.773(4) . ? Mo5 O6 1.774(5) . ? Mo5 O19 2.140(3) . ? Mo5 O17 2.144(4) . ? Mo5 O18 2.310(4) . ? N1 H1C 0.8899 . ? N1 H1D 0.8900 . ? N1 H1E 0.8901 . ? N1 H1F 0.9100 . ? N2 H2C 0.8898 . ? N2 H2D 0.8901 . ? N2 H2E 0.8901 . ? N2 H2F 0.9100 . ? O26 H26A 0.8502 . ? O26 H26B 0.8513 . ? O1 Mo1 1.934(3) 3_655 ? O5 V1 1.689(6) . ? O5 Mo1 2.307(4) 3_655 ? O10 V1 1.694(5) . ? O14 Mo3 1.9109(11) 3_655 ? O15 Mo3 2.228(5) 3_655 ? O18 V1 1.798(6) . ? O18 Mo5 2.310(4) 3_655 ? O19 Mo5 2.140(3) 3_655 ? O22 H22A 0.8477 . ? O22 H22B 0.9599 . ? O23 H23A 0.8499 . ? O23 H23B 0.8498 . ? O24 H24A 0.8500 . ? O24 H24B 0.8494 . ? O25 H25A 0.8500 . ? O25 H25B 0.8500 . ? N4 H4C 0.8901 . ? N4 H4D 0.8901 . ? N4 H4E 0.8901 . ? N4 H4F 0.9099 . ? V1 O10 1.694(5) 3_655 ?