#------------------------------------------------------------------------------ #$Date: 2023-11-02 04:30:41 +0200 (Thu, 02 Nov 2023) $ #$Revision: 287242 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/76/7247662.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_7247662 loop_ _publ_author_name 'George, Tanner' 'Brosseau, Christa L.' 'Masuda, Jason D.' _publ_section_title ; Electrochemical and X-ray structural evidence of multiple molybdenum precursor candidates from a reported non-aqueous electrodeposition of molybdenum disulfide ; _journal_issue 46 _journal_name_full 'RSC Advances' _journal_page_first 32199 _journal_page_last 32216 _journal_paper_doi 10.1039/D3RA04605B _journal_volume 13 _journal_year 2023 _chemical_formula_moiety 'C24 H54 Mo8 O32, 2(C2 H6 O2)' _chemical_formula_sum 'C28 H66 Mo8 O36' _chemical_formula_weight 1746.32 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2023-09-10 _audit_creation_method ; Olex2 1.5 (compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) ; _audit_update_record ; 2023-10-01 deposited with the CCDC. 2023-10-06 downloaded from the CCDC. ; _cell_angle_alpha 81.706(2) _cell_angle_beta 77.862(2) _cell_angle_gamma 69.992(2) _cell_formula_units_Z 1 _cell_length_a 8.5318(4) _cell_length_b 11.0284(5) _cell_length_c 14.5245(7) _cell_measurement_reflns_used 9042 _cell_measurement_temperature 125.0 _cell_measurement_theta_max 33.82 _cell_measurement_theta_min 2.53 _cell_volume 1251.55(10) _computing_cell_refinement 'SAINT V8.40B (Bruker AXS Inc., 2016)' _computing_data_collection 'APEX4 (Bruker AXS Inc., 2021)' _computing_data_reduction 'SAINT V8.40B (Bruker AXS Inc., 2016)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 125.00 _diffrn_detector '100 \\times 140 mm^2^ CMOS sensor' _diffrn_detector_area_resol_mean 7.3910 _diffrn_detector_type 'Bruker PHOTON III' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device '\k--geometry diffractometer' _diffrn_measurement_device_type 'Bruker D8 VENTURE' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'multilayer mirror' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_unetI/netI 0.0176 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 126602 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 33.901 _diffrn_reflns_theta_min 2.347 _diffrn_source 'microfocus sealed tube' _diffrn_source_type 'Incoatec I\mS 3.0' _exptl_absorpt_coefficient_mu 2.040 _exptl_absorpt_correction_T_max 0.7467 _exptl_absorpt_correction_T_min 0.6864 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1101 before and 0.0533 after correction. The Ratio of minimum to maximum transmission is 0.9192. The \l/2 correction factor is Not present. ; _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 2.317 _exptl_crystal_description Blade _exptl_crystal_F_000 858 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _refine_diff_density_max 1.303 _refine_diff_density_min -1.205 _refine_diff_density_rms 0.114 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 355 _refine_ls_number_reflns 10104 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.078 _refine_ls_R_factor_all 0.0267 _refine_ls_R_factor_gt 0.0219 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0198P)^2^+1.9118P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.0554 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9085 _reflns_number_total 10104 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ra04605b2.cif _cod_data_source_block mo_2021_03_03_jdm_tg216a_0m_a _cod_database_code 7247662 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.923 _shelx_estimated_absorpt_t_min 0.792 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups, All C(H,H,H,H) groups 2. Restrained distances O18-H18 0.84 with sigma of 0.02 O14-C10A \\sim O14-C10B with sigma of 0.02 C9-C10A \\sim C9-C10B with sigma of 0.02 3. Others Sof(H9BC)=Sof(H9BD)=Sof(C10B)=Sof(H10C)=Sof(H10D)=1-FVAR(1) Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10A)=Sof(H10B)=FVAR(1) 4.a Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9AA,H9AB), C9(H9BC,H9BD), C11(H11A,H11B), C12(H12A,H12B), C10A(H10A,H10B), C10B(H10C,H10D), C13(H13A,H13B), C14(H14A, H14B) ; _shelx_res_file ; TITL mo_2021_03_03_JDM_TG216A_0m_a.res in P-1 mo_2021_03_03_jdm_tg216a_0m_a.res created by SHELXL-2018/3 at 23:29:02 on 10-Sep-2023 REM Old TITL mo_2021_03_03_JDM_TG216A_0m in P-1 REM SHELXT solution in P-1: R1 0.058, Rweak 0.004, Alpha 0.045 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C14 Mo4 O18 CELL 0.71073 8.5318 11.0284 14.5245 81.706 77.862 69.992 ZERR 1 0.0004 0.0005 0.0007 0.002 0.002 0.002 LATT 1 SFAC C H Mo O UNIT 28 66 8 36 EQIV $1 -1+X,1+Y,+Z EQIV $2 1-X,1-Y,1-Z SADI O14 C10A O14 C10B SADI C9 C10A C9 C10B DFIX 0.84 O18 H18 L.S. 10 PLAN 7 SIZE 0.04 0.07 0.12 TEMP -148.15 CONF HTAB O12 O8 HTAB O13 O17 HTAB O17 O12 HTAB O18 O4_$1 HTAB O16 O3_$2 BOND LIST 4 MORE -1 BOND $H fmap 2 acta OMIT -2 9 2 OMIT 3 4 1 OMIT 3 8 2 REM REM REM WGHT 0.019800 1.911800 FVAR 0.35025 0.71880 MO1 3 0.649792 0.095914 0.724513 11.00000 0.01751 0.01193 = 0.01588 0.00138 -0.00497 -0.00139 MO2 3 0.735975 0.293124 0.747670 11.00000 0.01211 0.01667 = 0.01556 0.00160 -0.00490 -0.00367 MO3 3 0.487941 0.397124 0.550957 11.00000 0.01213 0.01079 = 0.01211 0.00089 -0.00360 -0.00370 MO4 3 0.462845 0.600010 0.630296 11.00000 0.01350 0.01167 = 0.01268 0.00010 -0.00396 -0.00381 O1 4 0.801540 0.014605 0.639960 11.00000 0.02705 0.01920 = 0.02275 -0.00266 -0.00304 0.00177 O2 4 0.921064 0.278630 0.674041 11.00000 0.01576 0.03143 = 0.02697 -0.00083 -0.00158 -0.00814 O3 4 0.428798 0.103299 0.698785 11.00000 0.02662 0.01554 = 0.02260 0.00538 -0.01033 -0.01028 O4 4 0.599933 -0.040152 0.819604 11.00000 0.02830 0.01590 = 0.02257 0.00533 -0.00847 -0.00571 O5 4 0.586751 0.483489 0.740738 11.00000 0.01890 0.01519 = 0.01612 0.00046 -0.00786 -0.00570 O6 4 0.762932 0.345092 0.864831 11.00000 0.02164 0.02341 = 0.02076 0.00071 -0.01087 -0.00557 O7 4 0.822495 0.101886 0.806257 11.00000 0.01738 0.01942 = 0.01983 0.00217 -0.00710 0.00007 O8 4 0.529078 0.228993 0.842075 11.00000 0.01681 0.01648 = 0.01333 0.00188 -0.00386 -0.00307 O9 4 0.592230 0.275417 0.662771 11.00000 0.01641 0.01392 = 0.01472 0.00252 -0.00590 -0.00483 O10 4 0.661181 0.488085 0.541980 11.00000 0.01355 0.01357 = 0.01385 0.00059 -0.00452 -0.00366 O11 4 0.307094 0.492591 0.654532 11.00000 0.01306 0.01639 = 0.01479 -0.00057 -0.00202 -0.00585 O12 4 0.222692 0.411129 0.854357 11.00000 0.01803 0.02359 = 0.01840 0.00000 -0.00311 -0.00054 H12 2 0.309550 0.363675 0.847910 11.00000 0.03766 O13 4 0.266561 0.739459 0.719366 11.00000 0.01755 0.01507 = 0.01838 -0.00057 -0.00192 -0.00335 H13 2 0.225624 0.713555 0.781521 11.00000 0.03689 O14 4 0.325272 0.723315 0.541179 11.00000 0.02047 0.01330 = 0.01631 -0.00153 -0.00698 0.00089 O15 4 0.594598 0.707788 0.632485 11.00000 0.01877 0.01572 = 0.01746 -0.00017 -0.00446 -0.00780 O16 4 0.661649 0.731606 0.432372 11.00000 0.02368 0.01820 = 0.01804 0.00384 -0.00878 -0.01177 H16 2 0.640675 0.780629 0.390115 11.00000 0.04030 C1 1 0.374443 -0.004988 0.738039 11.00000 0.03630 0.02203 = 0.02983 0.00664 -0.01202 -0.01728 AFIX 23 H1A 2 0.425041 -0.076478 0.695773 11.00000 -1.20000 H1B 2 0.249576 0.019727 0.746583 11.00000 -1.20000 AFIX 0 C2 1 0.432298 -0.046037 0.831204 11.00000 0.03362 0.02649 = 0.02678 0.00836 -0.00650 -0.01489 AFIX 23 H2A 2 0.355663 0.012248 0.879382 11.00000 -1.20000 H2B 2 0.431634 -0.135358 0.852260 11.00000 -1.20000 AFIX 0 C3 1 0.613496 0.555405 0.808765 11.00000 0.02532 0.02034 = 0.02148 -0.00211 -0.01260 -0.00644 AFIX 23 H3A 2 0.512435 0.631831 0.824215 11.00000 -1.20000 H3B 2 0.712282 0.585290 0.783180 11.00000 -1.20000 AFIX 0 C4 1 0.644487 0.464506 0.894328 11.00000 0.02552 0.02767 = 0.02101 -0.00139 -0.00860 -0.00800 AFIX 23 H4A 2 0.689850 0.500369 0.937605 11.00000 -1.20000 H4B 2 0.537248 0.451515 0.928243 11.00000 -1.20000 AFIX 0 C5 1 0.769151 0.085996 0.906517 11.00000 0.02569 0.02155 = 0.01932 0.00473 -0.01059 -0.00286 AFIX 23 H5A 2 0.836922 0.116082 0.940163 11.00000 -1.20000 H5B 2 0.784616 -0.006358 0.926939 11.00000 -1.20000 AFIX 0 C6 1 0.579154 0.167794 0.928994 11.00000 0.02411 0.02037 = 0.01523 0.00378 -0.00597 -0.00420 AFIX 23 H6A 2 0.510567 0.111454 0.958727 11.00000 -1.20000 H6B 2 0.562868 0.233473 0.973013 11.00000 -1.20000 AFIX 0 C7 1 0.141338 0.492156 0.699814 11.00000 0.01203 0.01891 = 0.01878 0.00032 -0.00325 -0.00523 AFIX 23 H7A 2 0.082572 0.476078 0.653171 11.00000 -1.20000 H7B 2 0.075394 0.578257 0.723144 11.00000 -1.20000 AFIX 0 C8 1 0.147484 0.389976 0.781489 11.00000 0.01756 0.01968 = 0.02018 0.00095 -0.00130 -0.00566 AFIX 23 H8A 2 0.030916 0.389610 0.808282 11.00000 -1.20000 H8B 2 0.213222 0.303941 0.757989 11.00000 -1.20000 AFIX 0 C9 1 0.137496 0.829643 0.669116 11.00000 0.01720 0.01777 = 0.02265 -0.00219 -0.00330 -0.00031 PART 1 AFIX 23 H9AA 2 0.088956 0.913139 0.698531 21.00000 -1.20000 H9AB 2 0.045009 0.793977 0.670691 21.00000 -1.20000 AFIX 23 PART 2 H9BC 2 0.146631 0.917542 0.664133 -21.00000 -1.20000 H9BD 2 0.023719 0.832769 0.704507 -21.00000 -1.20000 AFIX 0 PART 0 C11 1 0.757567 0.701829 0.581641 11.00000 0.01771 0.02441 = 0.01905 0.00034 -0.00551 -0.01002 AFIX 23 H11A 2 0.825103 0.611078 0.569198 11.00000 -1.20000 H11B 2 0.817194 0.734243 0.619126 11.00000 -1.20000 AFIX 0 C12 1 0.738809 0.783451 0.489929 11.00000 0.02203 0.02458 = 0.01902 0.00051 -0.00470 -0.01508 AFIX 23 H12A 2 0.667652 0.873382 0.502663 11.00000 -1.20000 H12B 2 0.851488 0.785066 0.455672 11.00000 -1.20000 AFIX 0 PART 1 C10A 1 0.221740 0.848347 0.570529 21.00000 0.01942 0.01217 = 0.01655 -0.00042 -0.00338 -0.00055 AFIX 23 H10A 2 0.136189 0.889730 0.529128 21.00000 -1.20000 H10B 2 0.292111 0.904543 0.567081 21.00000 -1.20000 AFIX 0 PART 2 C10B 1 0.160682 0.785543 0.567282 -21.00000 0.01535 0.02419 = 0.02301 0.00162 -0.00361 -0.00426 AFIX 23 H10C 2 0.093711 0.727518 0.568302 -21.00000 -1.20000 H10D 2 0.122089 0.861699 0.522500 -21.00000 -1.20000 AFIX 0 PART 0 O17 4 0.188133 0.650116 0.888429 11.00000 0.01943 0.02629 = 0.02182 -0.00073 -0.00445 -0.00532 H17 2 0.188612 0.581485 0.882756 11.00000 0.03795 O18 4 -0.134850 0.737018 0.828240 11.00000 0.02456 0.02948 = 0.02420 -0.00274 -0.00877 0.00133 H18 2 -0.201921 0.805123 0.830444 11.00000 0.02316 C13 1 0.033659 0.712832 0.948620 11.00000 0.02282 0.02910 = 0.01993 -0.00454 -0.00382 -0.00244 AFIX 23 H13A 2 0.017137 0.806670 0.944379 11.00000 -1.20000 H13B 2 0.042502 0.678412 1.014827 11.00000 -1.20000 AFIX 0 C14 1 -0.116950 0.693743 0.923264 11.00000 0.02069 0.02700 = 0.02346 0.00172 -0.00293 -0.00301 AFIX 23 H14A 2 -0.105756 0.600652 0.933544 11.00000 -1.20000 H14B 2 -0.220380 0.741446 0.965535 11.00000 -1.20000 AFIX 0 HKLF 4 REM mo_2021_03_03_JDM_TG216A_0m_a.res in P-1 REM wR2 = 0.0554, GooF = S = 1.075, Restrained GooF = 1.078 for all data REM R1 = 0.0219 for 9085 Fo > 4sig(Fo) and 0.0267 for all 10104 data REM 355 parameters refined using 3 restraints END WGHT 0.0198 1.9151 REM Highest difference peak 1.303, deepest hole -1.205, 1-sigma level 0.114 Q1 1 0.6970 0.3264 0.7820 11.00000 0.05 1.30 Q2 1 0.7463 0.4842 0.8602 11.00000 0.05 0.78 Q3 1 0.4767 0.5976 0.5709 11.00000 0.05 0.76 Q4 1 0.7409 0.0361 0.6796 11.00000 0.05 0.68 Q5 1 0.6065 0.5187 0.8566 11.00000 0.05 0.66 Q6 1 0.4166 -0.0311 0.7811 11.00000 0.05 0.62 Q7 1 0.3185 0.0411 0.7803 11.00000 0.05 0.62 ; _shelx_res_checksum 78360 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.64979(2) 0.09591(2) 0.72451(2) 0.01592(3) Uani 1 1 d . . . . . Mo2 Mo 0.73598(2) 0.29312(2) 0.74767(2) 0.01495(3) Uani 1 1 d . . . . . Mo3 Mo 0.48794(2) 0.39712(2) 0.55096(2) 0.01163(3) Uani 1 1 d . . . . . Mo4 Mo 0.46284(2) 0.60001(2) 0.63030(2) 0.01253(3) Uani 1 1 d . . . . . O1 O 0.8015(2) 0.01461(14) 0.63996(11) 0.0255(3) Uani 1 1 d . . . . . O2 O 0.92106(18) 0.27863(16) 0.67404(11) 0.0251(3) Uani 1 1 d . . . . . O3 O 0.42880(19) 0.10330(13) 0.69879(10) 0.0205(3) Uani 1 1 d . . . . . O4 O 0.5999(2) -0.04015(14) 0.81960(11) 0.0227(3) Uani 1 1 d . . . . . O5 O 0.58675(17) 0.48349(12) 0.74074(9) 0.0161(2) Uani 1 1 d . . . . . O6 O 0.76293(19) 0.34509(14) 0.86483(10) 0.0215(3) Uani 1 1 d . . . . . O7 O 0.82249(18) 0.10189(14) 0.80626(10) 0.0202(3) Uani 1 1 d . . . . . O8 O 0.52908(17) 0.22899(13) 0.84208(9) 0.0163(2) Uani 1 1 d . . . . . O9 O 0.59223(16) 0.27542(12) 0.66277(9) 0.0149(2) Uani 1 1 d . . . . . O10 O 0.66118(16) 0.48808(12) 0.54198(9) 0.0137(2) Uani 1 1 d . . . . . O11 O 0.30709(16) 0.49259(12) 0.65453(9) 0.0146(2) Uani 1 1 d . . . . . O12 O 0.22269(19) 0.41113(15) 0.85436(10) 0.0218(3) Uani 1 1 d . . . . . H12 H 0.310(4) 0.364(3) 0.848(2) 0.038(9) Uiso 1 1 d . . . . . O13 O 0.26656(17) 0.73946(13) 0.71937(10) 0.0178(2) Uani 1 1 d . . . . . H13 H 0.226(4) 0.714(3) 0.782(2) 0.037(8) Uiso 1 1 d . . . . . O14 O 0.32527(18) 0.72331(12) 0.54118(9) 0.0177(2) Uani 1 1 d D . . . . O15 O 0.59460(17) 0.70779(13) 0.63249(9) 0.0166(2) Uani 1 1 d . . . . . O16 O 0.66165(18) 0.73161(14) 0.43237(10) 0.0184(2) Uani 1 1 d . . . . . H16 H 0.641(4) 0.781(3) 0.390(2) 0.040(9) Uiso 1 1 d . . . . . C1 C 0.3744(3) -0.0050(2) 0.73804(16) 0.0272(4) Uani 1 1 d . . . . . H1A H 0.425041 -0.076478 0.695773 0.033 Uiso 1 1 calc R U . . . H1B H 0.249576 0.019727 0.746583 0.033 Uiso 1 1 calc R U . . . C2 C 0.4323(3) -0.0460(2) 0.83120(16) 0.0285(4) Uani 1 1 d . . . . . H2A H 0.355663 0.012248 0.879382 0.034 Uiso 1 1 calc R U . . . H2B H 0.431634 -0.135358 0.852260 0.034 Uiso 1 1 calc R U . . . C3 C 0.6135(3) 0.55541(19) 0.80877(14) 0.0212(3) Uani 1 1 d . . . . . H3A H 0.512435 0.631831 0.824215 0.025 Uiso 1 1 calc R U . . . H3B H 0.712282 0.585290 0.783180 0.025 Uiso 1 1 calc R U . . . C4 C 0.6445(3) 0.4645(2) 0.89433(15) 0.0242(4) Uani 1 1 d . . . . . H4A H 0.689850 0.500369 0.937605 0.029 Uiso 1 1 calc R U . . . H4B H 0.537248 0.451515 0.928243 0.029 Uiso 1 1 calc R U . . . C5 C 0.7692(3) 0.0860(2) 0.90652(14) 0.0231(4) Uani 1 1 d . . . . . H5A H 0.836922 0.116082 0.940163 0.028 Uiso 1 1 calc R U . . . H5B H 0.784616 -0.006358 0.926939 0.028 Uiso 1 1 calc R U . . . C6 C 0.5792(3) 0.16779(19) 0.92899(13) 0.0208(3) Uani 1 1 d . . . . . H6A H 0.510567 0.111454 0.958727 0.025 Uiso 1 1 calc R U . . . H6B H 0.562868 0.233473 0.973013 0.025 Uiso 1 1 calc R U . . . C7 C 0.1413(2) 0.49216(18) 0.69981(13) 0.0166(3) Uani 1 1 d . . . . . H7A H 0.082572 0.476078 0.653171 0.020 Uiso 1 1 calc R U . . . H7B H 0.075394 0.578257 0.723144 0.020 Uiso 1 1 calc R U . . . C8 C 0.1475(2) 0.38998(19) 0.78149(14) 0.0198(3) Uani 1 1 d . . . . . H8A H 0.030916 0.389610 0.808282 0.024 Uiso 1 1 calc R U . . . H8B H 0.213222 0.303941 0.757989 0.024 Uiso 1 1 calc R U . . . C9 C 0.1375(2) 0.82964(18) 0.66912(14) 0.0206(3) Uani 1 1 d D . . . . H9AA H 0.088956 0.913139 0.698531 0.025 Uiso 0.719(7) 1 calc R U P A 1 H9AB H 0.045009 0.793977 0.670691 0.025 Uiso 0.719(7) 1 calc R U P A 1 H9BC H 0.146631 0.917542 0.664133 0.025 Uiso 0.281(7) 1 calc R U P A 2 H9BD H 0.023719 0.832769 0.704507 0.025 Uiso 0.281(7) 1 calc R U P A 2 C11 C 0.7576(2) 0.70183(19) 0.58164(13) 0.0194(3) Uani 1 1 d . . . . . H11A H 0.825103 0.611078 0.569198 0.023 Uiso 1 1 calc R U . . . H11B H 0.817194 0.734243 0.619126 0.023 Uiso 1 1 calc R U . . . C12 C 0.7388(3) 0.7835(2) 0.48993(13) 0.0199(3) Uani 1 1 d . . . . . H12A H 0.667652 0.873382 0.502663 0.024 Uiso 1 1 calc R U . . . H12B H 0.851488 0.785066 0.455672 0.024 Uiso 1 1 calc R U . . . C10A C 0.2217(3) 0.8483(2) 0.57053(18) 0.0173(6) Uani 0.719(7) 1 d D . P A 1 H10A H 0.136189 0.889730 0.529128 0.021 Uiso 0.719(7) 1 calc R U P A 1 H10B H 0.292111 0.904543 0.567081 0.021 Uiso 0.719(7) 1 calc R U P A 1 C10B C 0.1607(8) 0.7855(7) 0.5673(5) 0.0217(16) Uani 0.281(7) 1 d D . P A 2 H10C H 0.093711 0.727518 0.568302 0.026 Uiso 0.281(7) 1 calc R U P A 2 H10D H 0.122089 0.861699 0.522500 0.026 Uiso 0.281(7) 1 calc R U P A 2 O17 O 0.18813(19) 0.65012(16) 0.88843(11) 0.0230(3) Uani 1 1 d . . . . . H17 H 0.189(4) 0.581(3) 0.883(2) 0.038(9) Uiso 1 1 d . . . . . O18 O -0.1349(2) 0.73702(17) 0.82824(12) 0.0279(3) Uani 1 1 d D . . . . H18 H -0.202(3) 0.8051(19) 0.830(2) 0.023(7) Uiso 1 1 d D . . . . C13 C 0.0337(3) 0.7128(2) 0.94862(15) 0.0252(4) Uani 1 1 d . . . . . H13A H 0.017137 0.806670 0.944379 0.030 Uiso 1 1 calc R U . . . H13B H 0.042502 0.678412 1.014827 0.030 Uiso 1 1 calc R U . . . C14 C -0.1170(3) 0.6937(2) 0.92326(15) 0.0255(4) Uani 1 1 d . . . . . H14A H -0.105756 0.600652 0.933544 0.031 Uiso 1 1 calc R U . . . H14B H -0.220380 0.741446 0.965535 0.031 Uiso 1 1 calc R 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 0.01751(7) 0.01193(6) 0.01588(7) 0.00138(5) -0.00497(5) -0.00139(5) Mo2 0.01211(6) 0.01667(6) 0.01556(6) 0.00160(5) -0.00490(5) -0.00367(5) Mo3 0.01213(6) 0.01079(6) 0.01211(6) 0.00089(4) -0.00360(4) -0.00370(4) Mo4 0.01350(6) 0.01167(6) 0.01268(6) 0.00010(4) -0.00396(4) -0.00381(5) O1 0.0270(7) 0.0192(6) 0.0227(7) -0.0027(5) -0.0030(6) 0.0018(5) O2 0.0158(6) 0.0314(8) 0.0270(7) -0.0008(6) -0.0016(5) -0.0081(6) O3 0.0266(7) 0.0155(6) 0.0226(6) 0.0054(5) -0.0103(5) -0.0103(5) O4 0.0283(7) 0.0159(6) 0.0226(7) 0.0053(5) -0.0085(6) -0.0057(5) O5 0.0189(6) 0.0152(5) 0.0161(5) 0.0005(4) -0.0079(5) -0.0057(5) O6 0.0216(6) 0.0234(6) 0.0208(6) 0.0007(5) -0.0109(5) -0.0056(5) O7 0.0174(6) 0.0194(6) 0.0198(6) 0.0022(5) -0.0071(5) 0.0001(5) O8 0.0168(6) 0.0165(5) 0.0133(5) 0.0019(4) -0.0039(4) -0.0031(5) O9 0.0164(5) 0.0139(5) 0.0147(5) 0.0025(4) -0.0059(4) -0.0048(4) O10 0.0136(5) 0.0136(5) 0.0138(5) 0.0006(4) -0.0045(4) -0.0037(4) O11 0.0131(5) 0.0164(5) 0.0148(5) -0.0006(4) -0.0020(4) -0.0058(4) O12 0.0180(6) 0.0236(7) 0.0184(6) 0.0000(5) -0.0031(5) -0.0005(5) O13 0.0176(6) 0.0151(5) 0.0184(6) -0.0006(5) -0.0019(5) -0.0033(5) O14 0.0205(6) 0.0133(5) 0.0163(6) -0.0015(4) -0.0070(5) 0.0009(5) O15 0.0188(6) 0.0157(5) 0.0175(6) -0.0002(4) -0.0045(5) -0.0078(5) O16 0.0237(6) 0.0182(6) 0.0180(6) 0.0038(5) -0.0088(5) -0.0118(5) C1 0.0363(11) 0.0220(9) 0.0298(10) 0.0066(8) -0.0120(9) -0.0173(8) C2 0.0336(11) 0.0265(10) 0.0268(10) 0.0084(8) -0.0065(8) -0.0149(9) C3 0.0253(9) 0.0203(8) 0.0215(8) -0.0021(7) -0.0126(7) -0.0064(7) C4 0.0255(9) 0.0277(9) 0.0210(9) -0.0014(7) -0.0086(7) -0.0080(8) C5 0.0257(9) 0.0216(8) 0.0193(8) 0.0047(7) -0.0106(7) -0.0029(7) C6 0.0241(9) 0.0204(8) 0.0152(7) 0.0038(6) -0.0060(6) -0.0042(7) C7 0.0120(7) 0.0189(7) 0.0188(7) 0.0003(6) -0.0033(6) -0.0052(6) C8 0.0176(8) 0.0197(8) 0.0202(8) 0.0010(6) -0.0013(6) -0.0057(6) C9 0.0172(8) 0.0178(8) 0.0227(8) -0.0022(6) -0.0033(6) -0.0003(6) C11 0.0177(8) 0.0244(8) 0.0191(8) 0.0003(6) -0.0055(6) -0.0100(7) C12 0.0220(8) 0.0246(8) 0.0190(8) 0.0005(6) -0.0047(6) -0.0151(7) C10A 0.0194(11) 0.0122(10) 0.0166(11) -0.0004(8) -0.0034(8) -0.0006(8) C10B 0.015(3) 0.024(3) 0.023(3) 0.002(2) -0.004(2) -0.004(2) O17 0.0194(6) 0.0263(7) 0.0218(7) -0.0007(6) -0.0045(5) -0.0053(6) O18 0.0246(7) 0.0295(8) 0.0242(7) -0.0027(6) -0.0088(6) 0.0013(6) C13 0.0228(9) 0.0291(10) 0.0199(8) -0.0045(7) -0.0038(7) -0.0024(8) C14 0.0207(9) 0.0270(9) 0.0235(9) 0.0017(7) -0.0029(7) -0.0030(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 Mo2 105.85(6) . . ? O1 Mo1 O3 107.91(7) . . ? O1 Mo1 O4 104.95(7) . . ? O1 Mo1 O7 94.13(7) . . ? O1 Mo1 O8 158.28(7) . . ? O1 Mo1 O9 100.88(6) . . ? O3 Mo1 Mo2 126.04(4) . . ? O3 Mo1 O4 79.64(6) . . ? O3 Mo1 O7 156.46(6) . . ? O3 Mo1 O8 92.67(6) . . ? O3 Mo1 O9 84.03(5) . . ? O4 Mo1 Mo2 129.13(4) . . ? O4 Mo1 O7 86.89(6) . . ? O4 Mo1 O8 85.12(6) . . ? O4 Mo1 O9 152.65(6) . . ? O7 Mo1 Mo2 51.56(4) . . ? O7 Mo1 O8 66.82(5) . . ? O8 Mo1 Mo2 54.52(3) . . ? O9 Mo1 Mo2 48.87(4) . . ? O9 Mo1 O7 100.20(5) . . ? O9 Mo1 O8 73.82(5) . . ? O2 Mo2 Mo1 105.77(6) . . ? O2 Mo2 O5 108.66(7) . . ? O2 Mo2 O6 105.28(7) . . ? O2 Mo2 O7 92.68(7) . . ? O2 Mo2 O8 157.64(7) . . ? O2 Mo2 O9 102.12(7) . . ? O5 Mo2 Mo1 126.01(4) . . ? O5 Mo2 O7 157.07(6) . . ? O5 Mo2 O8 92.98(5) . . ? O6 Mo2 Mo1 128.15(4) . . ? O6 Mo2 O5 79.91(6) . . ? O6 Mo2 O7 86.56(6) . . ? O6 Mo2 O8 83.53(6) . . ? O6 Mo2 O9 151.30(6) . . ? O7 Mo2 Mo1 51.66(4) . . ? O7 Mo2 O8 66.98(5) . . ? O8 Mo2 Mo1 54.73(3) . . ? O9 Mo2 Mo1 49.21(4) . . ? O9 Mo2 O5 83.43(5) . . ? O9 Mo2 O7 100.62(5) . . ? O9 Mo2 O8 74.14(5) . . ? Mo3 Mo3 Mo4 60.380(7) 2_666 2_666 ? Mo3 Mo3 Mo4 59.896(7) 2_666 . ? Mo4 Mo3 Mo4 120.276(7) 2_666 . ? O9 Mo3 Mo3 138.90(4) . 2_666 ? O9 Mo3 Mo4 91.05(4) . . ? O9 Mo3 Mo4 137.21(4) . 2_666 ? O9 Mo3 O16 83.10(5) . 2_666 ? O10 Mo3 Mo3 51.10(3) . 2_666 ? O10 Mo3 Mo3 50.54(3) 2_666 2_666 ? O10 Mo3 Mo4 90.61(4) . 2_666 ? O10 Mo3 Mo4 50.63(4) . . ? O10 Mo3 Mo4 89.89(4) 2_666 . ? O10 Mo3 Mo4 50.76(4) 2_666 2_666 ? O10 Mo3 O9 88.33(5) . . ? O10 Mo3 O9 167.77(5) 2_666 . ? O10 Mo3 O10 101.64(4) . 2_666 ? O10 Mo3 O11 99.94(5) . . ? O10 Mo3 O14 99.75(5) 2_666 2_666 ? O10 Mo3 O14 83.90(5) . 2_666 ? O10 Mo3 O16 87.63(5) 2_666 2_666 ? O10 Mo3 O16 169.61(5) . 2_666 ? O11 Mo3 Mo3 95.13(4) . 2_666 ? O11 Mo3 Mo4 137.39(4) . 2_666 ? O11 Mo3 Mo4 49.94(4) . . ? O11 Mo3 O9 84.66(5) . . ? O11 Mo3 O10 86.63(5) . 2_666 ? O11 Mo3 O14 171.80(5) . 2_666 ? O11 Mo3 O16 85.12(5) . 2_666 ? O14 Mo3 Mo3 92.91(4) 2_666 2_666 ? O14 Mo3 Mo4 49.18(4) 2_666 2_666 ? O14 Mo3 Mo4 134.51(4) 2_666 . ? O14 Mo3 O9 88.24(5) 2_666 . ? O14 Mo3 O16 89.98(6) 2_666 2_666 ? O16 Mo3 Mo3 137.95(4) 2_666 2_666 ? O16 Mo3 Mo4 91.72(4) 2_666 2_666 ? O16 Mo3 Mo4 135.06(4) 2_666 . ? Mo3 Mo4 Mo3 59.724(6) 2_666 . ? O5 Mo4 Mo3 135.99(4) . 2_666 ? O5 Mo4 Mo3 91.44(4) . . ? O5 Mo4 O13 96.69(5) . . ? O10 Mo4 Mo3 50.96(3) . 2_666 ? O10 Mo4 Mo3 50.26(3) . . ? O10 Mo4 O5 85.17(5) . . ? O10 Mo4 O13 172.44(5) . . ? O11 Mo4 Mo3 95.41(4) . 2_666 ? O11 Mo4 Mo3 50.51(4) . . ? O11 Mo4 O5 88.28(5) . . ? O11 Mo4 O10 100.15(5) . . ? O11 Mo4 O13 87.26(5) . . ? O13 Mo4 Mo3 127.25(4) . 2_666 ? O13 Mo4 Mo3 136.76(4) . . ? O14 Mo4 Mo3 51.90(4) . 2_666 ? O14 Mo4 Mo3 94.31(4) . . ? O14 Mo4 O5 172.11(5) . . ? O14 Mo4 O10 102.67(5) . . ? O14 Mo4 O11 91.21(6) . . ? O14 Mo4 O13 75.42(5) . . ? O15 Mo4 Mo3 95.41(4) . 2_666 ? O15 Mo4 Mo3 138.90(4) . . ? O15 Mo4 O5 85.71(5) . . ? O15 Mo4 O10 88.67(5) . . ? O15 Mo4 O11 168.88(5) . . ? O15 Mo4 O13 84.17(6) . . ? O15 Mo4 O14 93.46(6) . . ? C1 O3 Mo1 115.32(12) . . ? C2 O4 Mo1 115.14(12) . . ? Mo2 O5 Mo4 130.49(6) . . ? C3 O5 Mo2 111.97(11) . . ? C3 O5 Mo4 114.72(11) . . ? C4 O6 Mo2 115.11(11) . . ? Mo2 O7 Mo1 76.78(4) . . ? C5 O7 Mo1 114.91(12) . . ? C5 O7 Mo2 114.26(12) . . ? Mo2 O8 Mo1 70.76(4) . . ? C6 O8 Mo1 111.23(11) . . ? C6 O8 Mo2 111.14(11) . . ? Mo1 O9 Mo3 144.97(7) . . ? Mo2 O9 Mo1 81.92(5) . . ? Mo2 O9 Mo3 132.07(6) . . ? Mo3 O10 Mo3 78.36(4) . 2_666 ? Mo3 O10 Mo4 79.11(5) . . ? Mo4 O10 Mo3 78.28(4) . 2_666 ? Mo4 O11 Mo3 79.55(5) . . ? C7 O11 Mo3 136.26(11) . . ? C7 O11 Mo4 142.71(11) . . ? C8 O12 H12 105(3) . . ? Mo4 O13 H13 120.2(19) . . ? C9 O13 Mo4 113.47(11) . . ? C9 O13 H13 114(2) . . ? Mo4 O14 Mo3 78.92(5) . 2_666 ? C10A O14 Mo3 152.36(14) . 2_666 ? C10A O14 Mo4 118.58(13) . . ? C10B O14 Mo4 121.8(3) . . ? C11 O15 Mo4 129.43(12) . . ? Mo3 O16 H16 109(3) 2_666 . ? C12 O16 Mo3 138.84(11) . 2_666 ? C12 O16 H16 108(3) . . ? O3 C1 H1A 110.4 . . ? O3 C1 H1B 110.4 . . ? O3 C1 C2 106.63(17) . . ? H1A C1 H1B 108.6 . . ? C2 C1 H1A 110.4 . . ? C2 C1 H1B 110.4 . . ? O4 C2 C1 107.78(18) . . ? O4 C2 H2A 110.1 . . ? O4 C2 H2B 110.1 . . ? C1 C2 H2A 110.1 . . ? C1 C2 H2B 110.1 . . ? H2A C2 H2B 108.5 . . ? O5 C3 H3A 110.5 . . ? O5 C3 H3B 110.5 . . ? O5 C3 C4 106.15(16) . . ? H3A C3 H3B 108.7 . . ? C4 C3 H3A 110.5 . . ? C4 C3 H3B 110.5 . . ? O6 C4 C3 108.09(17) . . ? O6 C4 H4A 110.1 . . ? O6 C4 H4B 110.1 . . ? C3 C4 H4A 110.1 . . ? C3 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? O7 C5 H5A 110.2 . . ? O7 C5 H5B 110.2 . . ? O7 C5 C6 107.37(14) . . ? H5A C5 H5B 108.5 . . ? C6 C5 H5A 110.2 . . ? C6 C5 H5B 110.2 . . ? O8 C6 C5 107.20(15) . . ? O8 C6 H6A 110.3 . . ? O8 C6 H6B 110.3 . . ? C5 C6 H6A 110.3 . . ? C5 C6 H6B 110.3 . . ? H6A C6 H6B 108.5 . . ? O11 C7 H7A 109.2 . . ? O11 C7 H7B 109.2 . . ? O11 C7 C8 111.84(14) . . ? H7A C7 H7B 107.9 . . ? C8 C7 H7A 109.2 . . ? C8 C7 H7B 109.2 . . ? O12 C8 C7 112.39(16) . . ? O12 C8 H8A 109.1 . . ? O12 C8 H8B 109.1 . . ? C7 C8 H8A 109.1 . . ? C7 C8 H8B 109.1 . . ? H8A C8 H8B 107.9 . . ? O13 C9 H9AA 110.4 . . ? O13 C9 H9AB 110.4 . . ? O13 C9 H9BC 109.7 . . ? O13 C9 H9BD 109.7 . . ? O13 C9 C10A 106.73(16) . . ? O13 C9 C10B 109.9(3) . . ? H9AA C9 H9AB 108.6 . . ? H9BC C9 H9BD 108.2 . . ? C10A C9 H9AA 110.4 . . ? C10A C9 H9AB 110.4 . . ? C10B C9 H9BC 109.7 . . ? C10B C9 H9BD 109.7 . . ? O15 C11 H11A 109.9 . . ? O15 C11 H11B 109.9 . . ? O15 C11 C12 108.83(15) . . ? H11A C11 H11B 108.3 . . ? C12 C11 H11A 109.9 . . ? C12 C11 H11B 109.9 . . ? O16 C12 C11 110.13(15) . . ? O16 C12 H12A 109.6 . . ? O16 C12 H12B 109.6 . . ? C11 C12 H12A 109.6 . . ? C11 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? O14 C10A C9 107.21(18) . . ? O14 C10A H10A 110.3 . . ? O14 C10A H10B 110.3 . . ? C9 C10A H10A 110.3 . . ? C9 C10A H10B 110.3 . . ? H10A C10A H10B 108.5 . . ? O14 C10B C9 107.0(4) . . ? O14 C10B H10C 110.3 . . ? O14 C10B H10D 110.3 . . ? C9 C10B H10C 110.3 . . ? C9 C10B H10D 110.3 . . ? H10C C10B H10D 108.6 . . ? C13 O17 H17 108(3) . . ? C14 O18 H18 105(2) . . ? O17 C13 H13A 109.1 . . ? O17 C13 H13B 109.1 . . ? O17 C13 C14 112.52(18) . . ? H13A C13 H13B 107.8 . . ? C14 C13 H13A 109.1 . . ? C14 C13 H13B 109.1 . . ? O18 C14 C13 112.38(18) . . ? O18 C14 H14A 109.1 . . ? O18 C14 H14B 109.1 . . ? C13 C14 H14A 109.1 . . ? C13 C14 H14B 109.1 . . ? H14A C14 H14B 107.9 . . ? 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 Mo1 Mo2 2.6064(2) . ? Mo1 O1 1.6861(15) . ? Mo1 O3 1.9707(14) . ? Mo1 O4 1.9830(14) . ? Mo1 O7 2.0999(14) . ? Mo1 O8 2.2538(13) . ? Mo1 O9 1.9930(12) . ? Mo2 O2 1.6820(15) . ? Mo2 O5 2.0500(13) . ? Mo2 O6 1.9528(14) . ? Mo2 O7 2.0972(14) . ? Mo2 O8 2.2479(13) . ? Mo2 O9 1.9830(13) . ? Mo3 Mo3 2.5700(3) 2_666 ? Mo3 Mo4 2.5870(2) . ? Mo3 Mo4 2.5746(2) 2_666 ? Mo3 O9 2.0958(12) . ? Mo3 O10 2.0258(12) . ? Mo3 O10 2.0421(12) 2_666 ? Mo3 O11 2.0301(13) . ? Mo3 O14 2.0645(13) 2_666 ? Mo3 O16 2.1712(13) 2_666 ? Mo4 O5 2.1286(13) . ? Mo4 O10 2.0365(13) . ? Mo4 O11 2.0133(12) . ? Mo4 O13 2.1780(14) . ? Mo4 O14 1.9852(13) . ? Mo4 O15 1.9020(13) . ? O3 C1 1.427(2) . ? O4 C2 1.427(3) . ? O5 C3 1.450(2) . ? O6 C4 1.417(3) . ? O7 C5 1.436(2) . ? O8 C6 1.420(2) . ? O11 C7 1.430(2) . ? O12 H12 0.74(3) . ? O12 C8 1.430(2) . ? O13 H13 0.94(3) . ? O13 C9 1.454(2) . ? O14 C10A 1.429(3) . ? O14 C10B 1.334(7) . ? O15 C11 1.415(2) . ? O16 H16 0.77(3) . ? O16 C12 1.444(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C1 C2 1.494(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.489(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5 C6 1.552(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.510(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9AA 0.9900 . ? C9 H9AB 0.9900 . ? C9 H9BC 0.9900 . ? C9 H9BD 0.9900 . ? C9 C10A 1.481(3) . ? C9 C10B 1.575(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C11 C12 1.502(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C10A H10A 0.9900 . ? C10A H10B 0.9900 . ? C10B H10C 0.9900 . ? C10B H10D 0.9900 . ? O17 H17 0.77(3) . ? O17 C13 1.430(3) . ? O18 H18 0.773(17) . ? O18 C14 1.416(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 C14 1.496(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? 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 O12 H12 O8 0.74(3) 1.95(3) 2.686(2) 174(4) . yes O13 H13 O17 0.94(3) 1.62(3) 2.552(2) 170(3) . yes O16 H16 O3 0.77(3) 1.73(3) 2.4891(19) 174(4) 2_666 yes O17 H17 O12 0.77(3) 1.89(3) 2.657(2) 171(4) . yes O18 H18 O4 0.773(17) 1.963(18) 2.720(2) 166(3) 1_465 yes 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 Mo1 O3 C1 C2 36.0(2) . . . . ? Mo1 O4 C2 C1 31.6(2) . . . . ? Mo1 O7 C5 C6 -42.54(18) . . . . ? Mo1 O8 C6 C5 38.68(17) . . . . ? Mo2 O5 C3 C4 -35.81(18) . . . . ? Mo2 O6 C4 C3 -38.1(2) . . . . ? Mo2 O7 C5 C6 43.60(18) . . . . ? Mo2 O8 C6 C5 -38.09(17) . . . . ? Mo3 O11 C7 C8 86.34(19) . . . . ? Mo3 O14 C10A C9 -167.9(2) 2_666 . . . ? Mo3 O14 C10B C9 165.6(2) 2_666 . . . ? Mo3 O16 C12 C11 19.2(3) 2_666 . . . ? Mo4 O5 C3 C4 161.15(13) . . . . ? Mo4 O11 C7 C8 -113.68(18) . . . . ? Mo4 O13 C9 C10A -31.01(19) . . . . ? Mo4 O13 C9 C10B 9.4(3) . . . . ? Mo4 O14 C10A C9 -43.2(2) . . . . ? Mo4 O14 C10B C9 41.6(6) . . . . ? Mo4 O15 C11 C12 90.08(18) . . . . ? O3 C1 C2 O4 -41.7(2) . . . . ? O5 C3 C4 O6 46.5(2) . . . . ? O7 C5 C6 O8 -0.6(2) . . . . ? O11 C7 C8 O12 62.1(2) . . . . ? O13 C9 C10A O14 45.0(2) . . . . ? O13 C9 C10B O14 -29.5(5) . . . . ? O15 C11 C12 O16 -63.2(2) . . . . ? O17 C13 C14 O18 -56.9(2) . . . . ?