#------------------------------------------------------------------------------ #$Date: 2023-11-02 04:30:41 +0200 (Thu, 02 Nov 2023) $ #$Revision: 287242 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/76/7247664.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_7247664 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 'C16 H36 Mo4 O20' _chemical_formula_sum 'C16 H36 Mo4 O20' _chemical_formula_weight 932.21 _space_group_crystal_system orthorhombic _space_group_IT_number 33 _space_group_name_Hall 'P 2c -2n' _space_group_name_H-M_alt 'P n a 21' _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 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 34.2851(19) _cell_length_b 9.7131(5) _cell_length_c 8.4881(4) _cell_measurement_reflns_used 9843 _cell_measurement_temperature 125 _cell_measurement_theta_max 35.67 _cell_measurement_theta_min 2.68 _cell_volume 2826.7(3) _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 0.999 _diffrn_measured_fraction_theta_max 0.999 _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 0.0390 _diffrn_reflns_av_unetI/netI 0.0163 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 57 _diffrn_reflns_limit_h_min -57 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 281755 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 36.335 _diffrn_reflns_theta_min 2.179 _diffrn_source 'microfocus sealed tube' _diffrn_source_type 'Incoatec I\mS 3.0' _exptl_absorpt_coefficient_mu 1.819 _exptl_absorpt_correction_T_max 0.1100 _exptl_absorpt_correction_T_min 0.0655 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1031 before and 0.0592 after correction. The Ratio of minimum to maximum transmission is 0.5955. The \l/2 correction factor is Not present. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 2.191 _exptl_crystal_description prism _exptl_crystal_F_000 1840 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _refine_diff_density_max 1.508 _refine_diff_density_min -2.102 _refine_diff_density_rms 0.185 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.05(7) _refine_ls_extinction_coef 0.00076(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 439 _refine_ls_number_reflns 13707 _refine_ls_number_restraints 219 _refine_ls_restrained_S_all 1.081 _refine_ls_R_factor_all 0.0682 _refine_ls_R_factor_gt 0.0655 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0002P)^2^+20.8382P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1327 _refine_ls_wR_factor_ref 0.1339 _reflns_Friedel_coverage 0.899 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.998 _reflns_number_gt 13061 _reflns_number_total 13707 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ra04605b2.cif _cod_data_source_block mo_jasontemp2021_0m_a_pl _cod_database_code 7247664 _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 0.811 _shelx_estimated_absorpt_t_min 0.669 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.95(8) 0.05(8) 2. Fixed Uiso At 1.2 times of: All C(H,H) groups At 1.5 times of: All O(H) groups, All O(H,H) groups 3. Restrained distances O5-H5 0.87 with sigma of 0.01 C5-H5 1.922041 with sigma of 0.02 Mo2-H5 2.676213 with sigma of 0.02 O1A-C1 \\sim O1B-C1B with sigma of 0.02 C1B-C1A \\sim C1-C2A with sigma of 0.02 C1A-O2 \\sim O2-C2A with sigma of 0.02 O14A-C12A \\sim O14B-C12B with sigma of 0.02 C12B-C11B \\sim C12A-C11A with sigma of 0.02 C11A-O13 \\sim O13-C11B with sigma of 0.02 O17-C15A \\sim O17-C15B with sigma of 0.02 O18-C16A \\sim O18-C16B with sigma of 0.02 C15A-C16A \\sim C15B-C16B with sigma of 0.02 O17-C16A \\sim O17-C16B with sigma of 0.04 O18-C15A \\sim O18-C15B with sigma of 0.04 4. Uiso/Uaniso restraints and constraints O1A \\sim C1 \\sim C2A \\sim O1B \\sim C1A \\sim C1B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A O13 \\sim O13 \\sim O14A \\sim C11A \\sim C12A \\sim O14B \\sim C11B \\sim C12B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A C15A \\sim C16A \\sim C15B \\sim C16B: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A Uanis(O1B) = Uanis(O1A) 5. Rigid body (RIGU) restrains O2, O1A, C1, C2A, O1B, C1A, C1B with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C15A, C16A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C15B, C16B with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 6. Others Sof(O1A)=Sof(H1A)=Sof(C1)=Sof(H1B)=Sof(H1C)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=1- FVAR(1) Sof(O1B)=Sof(H1BA)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C1B)=Sof(H1BB)=Sof(H1BC)= FVAR(1) Sof(O14B)=Sof(H14D)=Sof(C11B)=Sof(H11C)=Sof(H11D)=Sof(C12B)=Sof(H12C)= Sof(H12D)=1-FVAR(2) Sof(O14A)=Sof(H14C)=Sof(C11A)=Sof(H11A)=Sof(H11B)=Sof(C12A)=Sof(H12A)= Sof(H12B)=FVAR(2) Sof(H17A)=Sof(C15B)=Sof(H15C)=Sof(H15D)=Sof(C16B)=Sof(H16C)=Sof(H16D)=1-FVAR(3) Sof(H17)=Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(C16A)=Sof(H16A)=Sof(H16B)=FVAR(3) 7.a Secondary CH2 refined with riding coordinates: C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C13(H13A,H13B), C14(H14A,H14B), C1(H1B,H1C), C2A(H2AA,H2AB), C11A(H11A,H11B), C12A(H12A,H12B), C15A(H15A,H15B), C16A(H16A, H16B), C1A(H1AA,H1AB), C1B(H1BB,H1BC), C11B(H11C,H11D), C12B(H12C,H12D), C15B(H15C,H15D), C16B(H16C,H16D) 7.b Tetrahedral OH refined with riding coordinates: O17(H17), O17(H17A) 7.c Idealised tetrahedral OH refined as rotating group: O1A(H1A), O14A(H14C), O1B(H1BA), O14B(H14D) ; _shelx_res_file ; TITL mo_jasonteP 1021_0m_a R = 0.18 New: Pna21 mo_jasontemp2021_0m_a_pl.res created by SHELXL-2018/3 at 22:06:01 on 10-Sep-2023 CELL 0.71073 34.2851 9.7131 8.4881 90 90 90 ZERR 4 0.0019 0.0005 0.0004 0 0 0 LATT -1 SYMM -X,-Y,0.5+Z SYMM 0.5-X,0.5+Y,0.5+Z SYMM 0.5+X,0.5-Y,+Z SFAC C H Mo O UNIT 64 144 16 80 EQIV $1 +X,+Y,1+Z EQIV $2 1-X,2-Y,0.5+Z EQIV $3 0.5-X,-0.5+Y,0.5+Z EQIV $4 +X,-1+Y,-1+Z SIMU O1A C1 C2A O1B C1A C1B SIMU O13 O13 O14A C11A C12A O14B C11B C12B EADP O1B O1A DFIX 0.87 0.01 O5 H5 DANG 1.922041 0.02 C5 H5 DANG 2.676213 0.02 Mo2 H5 RIGU O2 O1A C1 C2A O1B C1A C1B SADI O1A C1 O1B C1B SADI C1B C1A C1 C2A SADI C1A O2 O2 C2A SADI O14A C12A O14B C12B SADI C12B C11B C12A C11A SADI C11A O13 O13 C11B SADI O17 C15A O17 C15B SADI O18 C16A O18 C16B SADI C15A C16A C15B C16B SADI 0.04 O17 C16A O17 C16B SADI 0.04 O18 C15A O18 C15B RIGU C15A C16A RIGU C15B C16B SIMU 0.001 0.002 2 C15A C16A C15B C16B L.S. 30 PLAN 30 SIZE 0.12 0.12 0.24 TEMP -148.15 CONF HTAB O17 O11 HTAB O5 O4 HTAB O1A O7 HTAB O5 O18_$1 HTAB C5 O18_$1 HTAB C6 O14B_$2 HTAB C8 O1A_$3 HTAB C13 O10_$4 HTAB C14 O10_$4 HTAB O14A O15 FREE C16A O17 FREE O18 O17 MORE -1 BOND $H LIST 4 fmap 2 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 OMIT 17 1 -4 OMIT 17 1 4 REM REM REM WGHT 0.000200 20.838200 EXTI 0.000757 BASF 0.05363 FVAR 0.21640 0.49957 0.63048 0.54353 MO1 3 0.297330 0.913324 -0.056558 11.00000 0.03746 0.03630 = 0.07074 0.00215 -0.01811 -0.00514 MO2 3 0.355634 1.064081 0.063298 11.00000 0.03806 0.03020 = 0.05172 -0.01047 -0.00368 -0.00457 MO3 3 0.440549 0.793145 -0.437257 11.00000 0.04186 0.03518 = 0.05099 -0.00336 -0.01215 -0.01242 MO4 3 0.401533 0.572698 -0.551010 11.00000 0.03662 0.03248 = 0.05152 -0.01286 0.00586 -0.00877 O2 4 0.323061 1.093994 -0.128588 11.00000 0.05712 0.03715 = 0.06438 0.00413 -0.01700 -0.00812 O3 4 0.330689 0.883623 0.141587 11.00000 0.03137 0.03554 = 0.04483 -0.00369 -0.00225 -0.00584 O4 4 0.386671 0.814440 0.376274 11.00000 0.03070 0.03776 = 0.03442 -0.01000 0.00022 -0.00231 O5 4 0.403372 0.992720 0.160913 11.00000 0.03459 0.04465 = 0.03573 -0.00413 -0.00753 -0.00882 H5 2 0.408972 0.929171 0.230084 11.00000 -1.50000 O6 4 0.393631 1.177896 -0.039789 11.00000 0.05078 0.04080 = 0.05738 -0.00499 -0.00395 -0.01179 O7 4 0.284508 0.881506 -0.273885 11.00000 0.05300 0.04306 = 0.05740 0.00230 -0.02243 -0.00749 O8 4 0.289907 0.715684 -0.049838 11.00000 0.05640 0.04530 = 0.08748 0.00648 -0.04405 -0.01205 O9 4 0.257794 0.981911 0.026429 11.00000 0.03774 0.05563 = 0.06808 0.00741 -0.00347 0.00123 O10 4 0.332349 1.165444 0.192276 11.00000 0.05608 0.03403 = 0.07801 -0.01577 0.01266 -0.00334 O11 4 0.367121 0.880741 -0.123772 11.00000 0.04963 0.02957 = 0.03509 -0.00562 -0.00775 -0.00633 O12 4 0.393319 0.686834 -0.355620 11.00000 0.05832 0.03179 = 0.03668 -0.00402 -0.00620 -0.01348 O13 4 0.450596 0.673719 -0.625283 11.00000 0.02980 0.03922 = 0.07817 -0.00679 0.00913 -0.00689 O15 4 0.391017 0.529036 -0.769480 11.00000 0.04280 0.03644 = 0.04306 -0.01569 0.01188 -0.00541 O16 4 0.346256 0.542435 -0.536426 11.00000 0.04085 0.04644 = 0.04318 -0.02467 0.01165 -0.01771 O17 4 0.416013 0.952362 -0.336631 11.00000 0.07685 0.03349 = 0.04153 -0.01177 -0.00373 -0.02536 PART 1 AFIX 83 H17 2 0.399162 0.957780 -0.265058 41.00000 -1.50000 AFIX 83 PART 2 H17A 2 0.403522 0.958224 -0.251760 -41.00000 -1.50000 AFIX 0 PART 0 O18 4 0.465547 0.938608 -0.553176 11.00000 0.03852 0.04088 = 0.05954 -0.00568 -0.01024 -0.01501 O19 4 0.473581 0.731846 -0.308524 11.00000 0.05986 0.05401 = 0.07514 0.01678 -0.02869 -0.01813 O20 4 0.422579 0.435945 -0.466057 11.00000 0.05780 0.03949 = 0.07309 -0.00519 -0.00410 -0.00649 C3 1 0.318902 0.844932 0.296261 11.00000 0.03031 0.04163 = 0.03889 -0.01215 0.00668 0.00022 AFIX 23 H3A 2 0.313453 0.744861 0.298662 11.00000 -1.20000 H3B 2 0.294549 0.894031 0.324019 11.00000 -1.20000 AFIX 0 C4 1 0.349826 0.878303 0.415346 11.00000 0.03485 0.04197 = 0.03143 -0.01426 0.00598 -0.00161 AFIX 23 H4A 2 0.353319 0.979374 0.420601 11.00000 -1.20000 H4B 2 0.341278 0.846147 0.520500 11.00000 -1.20000 AFIX 0 C5 1 0.439252 1.049688 0.099280 11.00000 0.04393 0.05736 = 0.05589 -0.00210 0.00195 -0.01647 AFIX 23 H5A 2 0.449275 0.992238 0.011858 11.00000 -1.20000 H5B 2 0.459365 1.054298 0.182801 11.00000 -1.20000 AFIX 0 C6 1 0.429482 1.189278 0.042328 11.00000 0.04943 0.04835 = 0.07104 -0.01805 -0.00054 -0.01825 AFIX 23 H6A 2 0.426847 1.253683 0.132098 11.00000 -1.20000 H6B 2 0.450178 1.223931 -0.028688 11.00000 -1.20000 AFIX 0 C7 1 0.269245 0.750143 -0.310504 11.00000 0.05934 0.05276 = 0.05907 -0.01242 -0.01588 -0.01673 AFIX 23 H7A 2 0.287267 0.701672 -0.382808 11.00000 -1.20000 H7B 2 0.243840 0.760668 -0.364618 11.00000 -1.20000 AFIX 0 C8 1 0.263939 0.667077 -0.164413 11.00000 0.09315 0.05948 = 0.11593 0.02338 -0.06539 -0.02993 AFIX 23 H8A 2 0.236770 0.675711 -0.126159 11.00000 -1.20000 H8B 2 0.269183 0.568740 -0.186596 11.00000 -1.20000 AFIX 0 C9 1 0.387350 0.756317 -0.081915 11.00000 0.06645 0.03372 = 0.02881 0.00011 -0.01120 -0.00291 AFIX 23 H9A 2 0.378555 0.725849 0.023565 11.00000 -1.20000 H9B 2 0.415666 0.775527 -0.075684 11.00000 -1.20000 AFIX 0 C10 1 0.380578 0.644192 -0.196722 11.00000 0.06506 0.03145 = 0.04737 -0.00286 -0.00019 -0.01349 AFIX 23 H10A 2 0.395225 0.561152 -0.163953 11.00000 -1.20000 H10B 2 0.352486 0.620680 -0.198949 11.00000 -1.20000 AFIX 0 C13 1 0.351979 0.487836 -0.805560 11.00000 0.04326 0.04318 = 0.03534 -0.01752 0.00160 -0.01017 AFIX 23 H13A 2 0.352234 0.407533 -0.877381 11.00000 -1.20000 H13B 2 0.337880 0.564050 -0.858039 11.00000 -1.20000 AFIX 0 C14 1 0.332012 0.450602 -0.652783 11.00000 0.04351 0.05166 = 0.05036 -0.01974 0.00751 -0.01888 AFIX 23 H14A 2 0.303386 0.460097 -0.663591 11.00000 -1.20000 H14B 2 0.338045 0.354279 -0.623456 11.00000 -1.20000 AFIX 0 PART 1 O1A 4 0.298671 1.108369 -0.442472 -21.00000 0.14263 0.15423 = 0.12863 -0.00404 0.06150 0.05191 AFIX 147 H1A 2 0.314361 1.053541 -0.399570 -21.00000 -1.50000 AFIX 0 O14A 4 0.452675 0.537241 -0.964218 31.00000 0.04058 0.08505 = 0.05716 -0.00117 0.01505 -0.00206 AFIX 147 H14C 2 0.431794 0.529179 -0.913280 31.00000 -1.50000 AFIX 0 C1 1 0.285572 1.206282 -0.329420 -21.00000 0.11023 0.09910 = 0.06177 0.03187 0.03151 0.04837 AFIX 23 H1B 2 0.261373 1.172605 -0.278773 -21.00000 -1.20000 H1C 2 0.279634 1.294558 -0.382561 -21.00000 -1.20000 AFIX 0 C2A 1 0.315822 1.228182 -0.208890 -21.00000 0.10915 0.07513 = 0.08591 0.03245 0.02395 0.04598 AFIX 23 H2AA 2 0.306969 1.297716 -0.131474 -21.00000 -1.20000 H2AB 2 0.340126 1.261853 -0.258711 -21.00000 -1.20000 AFIX 0 C11A 1 0.481765 0.661378 -0.736175 31.00000 0.05040 0.09847 = 0.09448 -0.00448 0.01210 -0.02129 AFIX 23 H11A 2 0.486501 0.755296 -0.777253 31.00000 -1.20000 H11B 2 0.505178 0.636256 -0.674258 31.00000 -1.20000 AFIX 0 C12A 1 0.481590 0.575390 -0.865797 31.00000 0.05713 0.15652 = 0.11219 -0.09054 0.01594 -0.01059 AFIX 23 H12A 2 0.501913 0.613845 -0.936000 31.00000 -1.20000 H12B 2 0.492346 0.487433 -0.825979 31.00000 -1.20000 AFIX 0 C15A 1 0.423196 1.089590 -0.402205 41.00000 0.04254 0.03535 = 0.04472 -0.00568 -0.00394 -0.00814 AFIX 23 H15A 2 0.422508 1.161962 -0.320125 41.00000 -1.20000 H15B 2 0.404545 1.112700 -0.487225 41.00000 -1.20000 AFIX 0 C16A 1 0.464210 1.066378 -0.465175 41.00000 0.04249 0.03550 = 0.04480 -0.00533 -0.00415 -0.00818 AFIX 23 H16A 2 0.471761 1.143950 -0.534410 41.00000 -1.20000 H16B 2 0.482918 1.062324 -0.376453 41.00000 -1.20000 AFIX 0 PART 2 O1B 4 0.267133 1.269583 -0.214549 21.00000 0.14263 0.15423 = 0.12863 -0.00404 0.06150 0.05191 AFIX 147 H1BA 2 0.261841 1.194280 -0.258265 21.00000 -1.50000 AFIX 0 O14B 4 0.529866 0.604333 -0.700124 -31.00000 0.04046 0.13915 = 0.09451 0.01445 -0.00899 0.02069 AFIX 147 H14D 2 0.527297 0.665073 -0.630448 -31.00000 -1.50000 AFIX 0 C1A 1 0.327307 1.174410 -0.277403 21.00000 0.07109 0.04780 = 0.03723 -0.01217 -0.00322 0.00069 AFIX 23 H1AA 2 0.355174 1.191104 -0.301246 21.00000 -1.20000 H1AB 2 0.315381 1.124454 -0.366931 21.00000 -1.20000 AFIX 0 C1B 1 0.306636 1.306395 -0.248469 21.00000 0.12831 0.06561 = 0.06240 0.00866 0.01423 0.03915 AFIX 23 H1BB 2 0.318418 1.355859 -0.158275 21.00000 -1.20000 H1BC 2 0.307932 1.366275 -0.342707 21.00000 -1.20000 AFIX 0 C11B 1 0.469165 0.699937 -0.770159 -31.00000 0.02707 0.03539 = 0.07206 0.03263 -0.00340 0.00407 AFIX 23 H11C 2 0.450204 0.698998 -0.858116 -31.00000 -1.20000 H11D 2 0.482719 0.789924 -0.768575 -31.00000 -1.20000 AFIX 0 C12B 1 0.495622 0.592092 -0.783500 -31.00000 0.05077 0.07547 = 0.05036 0.02859 -0.02035 0.00837 AFIX 23 H12C 2 0.482439 0.506503 -0.749211 -31.00000 -1.20000 H12D 2 0.502253 0.580960 -0.896299 -31.00000 -1.20000 AFIX 0 C15B 1 0.442904 1.073129 -0.351550 -41.00000 0.04248 0.03539 = 0.04465 -0.00561 -0.00405 -0.00816 AFIX 23 H15C 2 0.428884 1.159455 -0.326291 -41.00000 -1.20000 H15D 2 0.465137 1.063437 -0.277954 -41.00000 -1.20000 AFIX 0 C16B 1 0.456872 1.076190 -0.514501 -41.00000 0.04272 0.03545 = 0.04466 -0.00560 -0.00416 -0.00811 AFIX 23 H16C 2 0.436509 1.113225 -0.585511 -41.00000 -1.20000 H16D 2 0.480461 1.134445 -0.523524 -41.00000 -1.20000 AFIX 0 HKLF 4 1 0 0 1 0 1 0 -1 0 0 REM mo_jasonteP 1021_0m_a R = 0.18 New: Pna21 REM wR2 = 0.1339, GooF = S = 1.084, Restrained GooF = 1.081 for all data REM R1 = 0.0655 for 13061 Fo > 4sig(Fo) and 0.0682 for all 13707 data REM 439 parameters refined using 219 restraints END WGHT 0.0000 20.3459 REM Highest difference peak 1.508, deepest hole -2.102, 1-sigma level 0.185 Q1 1 0.4435 0.5021 -0.4404 11.00000 0.05 1.51 Q2 1 0.4339 0.8030 -0.4118 11.00000 0.05 1.43 Q3 1 0.4460 0.7386 -0.4261 11.00000 0.05 1.39 Q4 1 0.3010 0.9339 -0.0015 11.00000 0.05 1.25 Q5 1 0.3992 0.6066 -0.3551 11.00000 0.05 1.21 Q6 1 0.2947 0.6257 -0.0407 11.00000 0.05 1.20 Q7 1 0.4740 1.2027 -0.4420 11.00000 0.05 1.18 Q8 1 0.4066 0.5660 -0.6163 11.00000 0.05 1.04 Q9 1 0.3416 1.1384 0.0552 11.00000 0.05 1.03 Q10 1 0.2992 1.1737 -0.0455 11.00000 0.05 1.01 Q11 1 0.4448 0.7831 -0.4903 11.00000 0.05 1.01 Q12 1 0.4343 1.0808 -0.4873 11.00000 0.05 0.95 Q13 1 0.3161 1.0426 -0.0489 11.00000 0.05 0.93 Q14 1 0.2876 1.3868 -0.0242 11.00000 0.05 0.85 Q15 1 0.3044 1.3247 -0.0604 11.00000 0.05 0.85 Q16 1 0.2446 0.9008 -0.4382 11.00000 0.05 0.84 Q17 1 0.4370 0.6243 -0.5015 11.00000 0.05 0.84 Q18 1 0.3048 0.9200 -0.0976 11.00000 0.05 0.81 Q19 1 0.3451 0.8428 0.0395 11.00000 0.05 0.81 Q20 1 0.4006 0.5161 -0.5301 11.00000 0.05 0.81 Q21 1 0.3419 0.3900 -0.9565 11.00000 0.05 0.81 Q22 1 0.4679 0.7198 -0.4560 11.00000 0.05 0.81 Q23 1 0.3551 0.3715 -0.8616 11.00000 0.05 0.80 Q24 1 0.3526 1.3452 -0.1756 11.00000 0.05 0.79 Q25 1 0.4010 0.8741 0.4015 11.00000 0.05 0.79 Q26 1 0.3807 0.8971 0.4591 11.00000 0.05 0.78 Q27 1 0.3895 0.6185 -0.8558 11.00000 0.05 0.76 Q28 1 0.4300 0.7164 -0.5207 11.00000 0.05 0.75 Q29 1 0.3385 1.0061 -0.0130 11.00000 0.05 0.75 Q30 1 0.2978 1.3670 -0.1432 11.00000 0.05 0.74 ; _shelx_res_checksum 84872 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, 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 0.29733(2) 0.91332(8) -0.05656(14) 0.0482(2) Uani 1 1 d . . . . . Mo2 Mo 0.35563(2) 1.06408(7) 0.06330(11) 0.03999(16) Uani 1 1 d D . . . . Mo3 Mo 0.44055(2) 0.79314(8) -0.43726(12) 0.04268(17) Uani 1 1 d . . . . . Mo4 Mo 0.40153(2) 0.57270(7) -0.55101(11) 0.04021(17) Uani 1 1 d . . . . . O2 O 0.3231(2) 1.0940(7) -0.1286(10) 0.0529(19) Uani 1 1 d D . . . . O3 O 0.33069(17) 0.8836(6) 0.1416(8) 0.0372(12) Uani 1 1 d . . . . . O4 O 0.38667(16) 0.8144(6) 0.3763(7) 0.0343(11) Uani 1 1 d . . . . . O5 O 0.40337(18) 0.9927(7) 0.1609(7) 0.0383(13) Uani 1 1 d D . . . . H5 H 0.4090(9) 0.929(9) 0.230(11) 0.057 Uiso 1 1 d D U . . . O6 O 0.3936(2) 1.1779(7) -0.0398(10) 0.0497(16) Uani 1 1 d . . . . . O7 O 0.2845(2) 0.8815(8) -0.2739(9) 0.0512(18) Uani 1 1 d . . . . . O8 O 0.2899(2) 0.7157(7) -0.0498(13) 0.063(2) Uani 1 1 d . . . . . O9 O 0.2578(2) 0.9819(8) 0.0264(10) 0.054(2) Uani 1 1 d . . . . . O10 O 0.3323(2) 1.1654(8) 0.1923(11) 0.056(2) Uani 1 1 d . . . . . O11 O 0.36712(19) 0.8807(6) -0.1238(7) 0.0381(13) Uani 1 1 d . . . . . O12 O 0.3933(2) 0.6868(6) -0.3556(8) 0.0423(15) Uani 1 1 d . . . . . O13 O 0.45060(18) 0.6737(7) -0.6253(10) 0.0491(18) Uani 1 1 d D U . . . O15 O 0.39102(19) 0.5290(7) -0.7695(8) 0.0408(14) Uani 1 1 d . . . . . O16 O 0.34626(17) 0.5424(7) -0.5364(8) 0.0435(15) Uani 1 1 d . . . . . O17 O 0.4160(2) 0.9524(7) -0.3366(9) 0.0506(18) Uani 1 1 d D . . . . H17 H 0.399162 0.957780 -0.265058 0.076 Uiso 0.544(17) 1 calc R U P A 1 H17A H 0.403522 0.958224 -0.251760 0.076 Uiso 0.456(17) 1 calc R U P A 2 O18 O 0.46555(17) 0.9386(7) -0.5532(10) 0.0463(14) Uani 1 1 d D . . . . O19 O 0.4736(3) 0.7318(9) -0.3085(11) 0.063(2) Uani 1 1 d . . . . . O20 O 0.4226(2) 0.4359(8) -0.4661(11) 0.057(2) Uani 1 1 d . . . . . C3 C 0.3189(2) 0.8449(9) 0.2963(10) 0.0369(17) Uani 1 1 d . . . . . H3A H 0.313453 0.744861 0.298662 0.044 Uiso 1 1 calc R U . . . H3B H 0.294549 0.894031 0.324019 0.044 Uiso 1 1 calc R U . . . C4 C 0.3498(2) 0.8783(9) 0.4153(9) 0.0361(16) Uani 1 1 d . . . . . H4A H 0.353319 0.979374 0.420601 0.043 Uiso 1 1 calc R U . . . H4B H 0.341278 0.846147 0.520500 0.043 Uiso 1 1 calc R U . . . C5 C 0.4393(3) 1.0497(12) 0.0993(14) 0.052(3) Uani 1 1 d D . . . . H5A H 0.449275 0.992238 0.011858 0.063 Uiso 1 1 calc R U . . . H5B H 0.459365 1.054298 0.182801 0.063 Uiso 1 1 calc R U . . . C6 C 0.4295(3) 1.1893(11) 0.0423(17) 0.056(3) Uani 1 1 d . . . . . H6A H 0.426847 1.253683 0.132098 0.068 Uiso 1 1 calc R U . . . H6B H 0.450178 1.223931 -0.028688 0.068 Uiso 1 1 calc R U . . . C7 C 0.2692(4) 0.7501(12) -0.3105(15) 0.057(3) Uani 1 1 d . . . . . H7A H 0.287267 0.701672 -0.382808 0.068 Uiso 1 1 calc R U . . . H7B H 0.243840 0.760668 -0.364618 0.068 Uiso 1 1 calc R U . . . C8 C 0.2639(5) 0.6671(15) -0.164(2) 0.090(6) Uani 1 1 d . . . . . H8A H 0.236770 0.675711 -0.126159 0.107 Uiso 1 1 calc R U . . . H8B H 0.269183 0.568740 -0.186596 0.107 Uiso 1 1 calc R U . . . C9 C 0.3874(3) 0.7563(9) -0.0819(10) 0.043(2) Uani 1 1 d . . . . . H9A H 0.378555 0.725849 0.023565 0.052 Uiso 1 1 calc R U . . . H9B H 0.415666 0.775527 -0.075684 0.052 Uiso 1 1 calc R U . . . C10 C 0.3806(3) 0.6442(10) -0.1967(12) 0.048(2) Uani 1 1 d . . . . . H10A H 0.395225 0.561152 -0.163953 0.058 Uiso 1 1 calc R U . . . H10B H 0.352486 0.620680 -0.198949 0.058 Uiso 1 1 calc R U . . . C13 C 0.3520(3) 0.4878(10) -0.8056(10) 0.0406(19) Uani 1 1 d . . . . . H13A H 0.352234 0.407533 -0.877381 0.049 Uiso 1 1 calc R U . . . H13B H 0.337880 0.564050 -0.858039 0.049 Uiso 1 1 calc R U . . . C14 C 0.3320(3) 0.4506(11) -0.6528(13) 0.049(2) Uani 1 1 d . . . . . H14A H 0.303386 0.460097 -0.663591 0.058 Uiso 1 1 calc R U . . . H14B H 0.338045 0.354279 -0.623456 0.058 Uiso 1 1 calc R U . . . O1A O 0.2987(10) 1.108(3) -0.442(4) 0.142(8) Uani 0.500(15) 1 d D U P B 1 H1A H 0.314361 1.053541 -0.399570 0.213 Uiso 0.500(15) 1 calc R U P B 1 O14A O 0.4527(3) 0.5372(16) -0.9642(16) 0.061(4) Uani 0.630(16) 1 d D U P C 1 H14C H 0.431794 0.529179 -0.913280 0.091 Uiso 0.630(16) 1 calc R U P C 1 C1 C 0.2856(10) 1.206(4) -0.329(3) 0.090(8) Uani 0.500(15) 1 d D U P B 1 H1B H 0.261373 1.172605 -0.278773 0.108 Uiso 0.500(15) 1 calc R U P B 1 H1C H 0.279634 1.294558 -0.382561 0.108 Uiso 0.500(15) 1 calc R U P B 1 C2A C 0.3158(10) 1.228(3) -0.209(4) 0.090(8) Uani 0.500(15) 1 d D U P B 1 H2AA H 0.306969 1.297716 -0.131474 0.108 Uiso 0.500(15) 1 calc R U P B 1 H2AB H 0.340126 1.261853 -0.258711 0.108 Uiso 0.500(15) 1 calc R U P B 1 C11A C 0.4818(7) 0.661(3) -0.736(3) 0.081(7) Uani 0.630(16) 1 d D U P C 1 H11A H 0.486501 0.755296 -0.777253 0.097 Uiso 0.630(16) 1 calc R U P C 1 H11B H 0.505178 0.636256 -0.674258 0.097 Uiso 0.630(16) 1 calc R U P C 1 C12A C 0.4816(7) 0.575(3) -0.866(3) 0.109(9) Uani 0.630(16) 1 d D U P C 1 H12A H 0.501913 0.613845 -0.936000 0.130 Uiso 0.630(16) 1 calc R U P C 1 H12B H 0.492346 0.487433 -0.825979 0.130 Uiso 0.630(16) 1 calc R U P C 1 C15A C 0.4232(5) 1.0896(15) -0.402(2) 0.041(2) Uani 0.544(17) 1 d D U P A 1 H15A H 0.422508 1.161962 -0.320125 0.049 Uiso 0.544(17) 1 calc R U P A 1 H15B H 0.404545 1.112700 -0.487225 0.049 Uiso 0.544(17) 1 calc R U P A 1 C16A C 0.4642(5) 1.0664(16) -0.465(2) 0.041(2) Uani 0.544(17) 1 d D U P A 1 H16A H 0.471761 1.143950 -0.534410 0.049 Uiso 0.544(17) 1 calc R U P A 1 H16B H 0.482918 1.062324 -0.376453 0.049 Uiso 0.544(17) 1 calc R U P A 1 O1B O 0.2671(10) 1.270(4) -0.215(4) 0.142(8) Uani 0.500(15) 1 d D U P B 2 H1BA H 0.261841 1.194280 -0.258265 0.213 Uiso 0.500(15) 1 calc R U P B 2 O14B O 0.5299(7) 0.604(4) -0.700(4) 0.091(11) Uani 0.370(16) 1 d D U P C 2 H14D H 0.527297 0.665073 -0.630448 0.137 Uiso 0.370(16) 1 calc R U P C 2 C1A C 0.3273(8) 1.174(2) -0.277(2) 0.052(5) Uani 0.500(15) 1 d D U P B 2 H1AA H 0.355174 1.191104 -0.301246 0.062 Uiso 0.500(15) 1 calc R U P B 2 H1AB H 0.315381 1.124454 -0.366931 0.062 Uiso 0.500(15) 1 calc R U P B 2 C1B C 0.3066(10) 1.306(3) -0.248(4) 0.085(7) Uani 0.500(15) 1 d D U P B 2 H1BB H 0.318418 1.355859 -0.158275 0.103 Uiso 0.500(15) 1 calc R U P B 2 H1BC H 0.307932 1.366275 -0.342707 0.103 Uiso 0.500(15) 1 calc R U P B 2 C11B C 0.4692(7) 0.700(3) -0.770(3) 0.045(6) Uani 0.370(16) 1 d D U P C 2 H11C H 0.450204 0.698998 -0.858116 0.054 Uiso 0.370(16) 1 calc R U P C 2 H11D H 0.482719 0.789924 -0.768575 0.054 Uiso 0.370(16) 1 calc R U P C 2 C12B C 0.4956(8) 0.592(3) -0.783(4) 0.059(8) Uani 0.370(16) 1 d D U P C 2 H12C H 0.482439 0.506503 -0.749211 0.071 Uiso 0.370(16) 1 calc R U P C 2 H12D H 0.502253 0.580960 -0.896299 0.071 Uiso 0.370(16) 1 calc R U P C 2 C15B C 0.4429(6) 1.0731(19) -0.352(2) 0.041(2) Uani 0.456(17) 1 d D U P A 2 H15C H 0.428884 1.159455 -0.326291 0.049 Uiso 0.456(17) 1 calc R U P A 2 H15D H 0.465137 1.063437 -0.277954 0.049 Uiso 0.456(17) 1 calc R U P A 2 C16B C 0.4569(7) 1.0762(18) -0.515(2) 0.041(2) Uani 0.456(17) 1 d D U P A 2 H16C H 0.436509 1.113225 -0.585511 0.049 Uiso 0.456(17) 1 calc R U P A 2 H16D H 0.480461 1.134445 -0.523524 0.049 Uiso 0.456(17) 1 calc R U P A 2 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 0.0375(3) 0.0363(3) 0.0707(6) 0.0021(4) -0.0181(4) -0.0051(3) Mo2 0.0381(3) 0.0302(3) 0.0517(4) -0.0105(3) -0.0037(4) -0.0046(2) Mo3 0.0419(3) 0.0352(3) 0.0510(4) -0.0034(4) -0.0122(4) -0.0124(3) Mo4 0.0366(3) 0.0325(3) 0.0515(4) -0.0129(3) 0.0059(3) -0.0088(2) O2 0.057(4) 0.037(3) 0.064(5) 0.004(3) -0.017(4) -0.008(3) O3 0.031(3) 0.036(3) 0.045(3) -0.004(2) -0.002(2) -0.006(2) O4 0.031(2) 0.038(3) 0.034(3) -0.010(2) 0.000(2) -0.002(2) O5 0.035(3) 0.045(3) 0.036(3) -0.004(3) -0.008(2) -0.009(2) O6 0.051(4) 0.041(3) 0.057(4) -0.005(4) -0.004(4) -0.012(3) O7 0.053(4) 0.043(4) 0.057(4) 0.002(3) -0.022(3) -0.007(3) O8 0.056(4) 0.045(4) 0.087(6) 0.006(4) -0.044(5) -0.012(3) O9 0.038(3) 0.056(4) 0.068(5) 0.007(4) -0.003(3) 0.001(3) O10 0.056(4) 0.034(3) 0.078(6) -0.016(4) 0.013(4) -0.003(3) O11 0.050(3) 0.030(3) 0.035(3) -0.006(2) -0.008(3) -0.006(2) O12 0.058(4) 0.032(3) 0.037(3) -0.004(2) -0.006(3) -0.013(3) O13 0.030(3) 0.039(3) 0.078(5) -0.007(3) 0.009(3) -0.007(2) O15 0.043(3) 0.036(3) 0.043(3) -0.016(3) 0.012(3) -0.005(2) O16 0.041(3) 0.046(3) 0.043(3) -0.025(3) 0.012(3) -0.018(2) O17 0.077(5) 0.033(3) 0.042(3) -0.012(3) -0.004(3) -0.025(3) O18 0.039(3) 0.041(3) 0.060(4) -0.006(4) -0.010(3) -0.015(2) O19 0.060(5) 0.054(5) 0.075(6) 0.017(4) -0.029(4) -0.018(4) O20 0.058(4) 0.039(3) 0.073(6) -0.005(4) -0.004(4) -0.006(3) C3 0.030(3) 0.042(4) 0.039(4) -0.012(3) 0.007(3) 0.000(3) C4 0.035(3) 0.042(4) 0.031(4) -0.014(3) 0.006(3) -0.002(3) C5 0.044(5) 0.057(6) 0.056(6) -0.002(5) 0.002(4) -0.016(4) C6 0.049(5) 0.048(5) 0.071(8) -0.018(6) -0.001(5) -0.018(4) C7 0.059(6) 0.053(6) 0.059(7) -0.012(5) -0.016(5) -0.017(5) C8 0.093(10) 0.059(8) 0.116(13) 0.023(8) -0.065(10) -0.030(7) C9 0.066(6) 0.034(4) 0.029(4) 0.000(3) -0.011(4) -0.003(4) C10 0.065(6) 0.031(4) 0.047(5) -0.003(4) 0.000(5) -0.013(4) C13 0.043(4) 0.043(4) 0.035(4) -0.018(3) 0.002(3) -0.010(4) C14 0.044(5) 0.052(5) 0.050(5) -0.020(4) 0.008(4) -0.019(4) O1A 0.143(14) 0.154(18) 0.129(15) -0.004(14) 0.062(13) 0.052(13) O14A 0.041(6) 0.085(10) 0.057(8) -0.001(7) 0.015(5) -0.002(6) C1 0.110(18) 0.099(17) 0.062(12) 0.032(11) 0.032(11) 0.048(15) C2A 0.109(18) 0.075(14) 0.086(15) 0.032(11) 0.024(13) 0.046(13) C11A 0.050(12) 0.098(19) 0.094(17) -0.004(15) 0.012(12) -0.021(12) C12A 0.057(12) 0.16(2) 0.112(18) -0.091(16) 0.016(12) -0.011(14) C15A 0.043(4) 0.035(3) 0.045(6) -0.006(4) -0.004(3) -0.008(4) C16A 0.042(4) 0.035(3) 0.045(6) -0.005(4) -0.004(3) -0.008(4) O1B 0.143(14) 0.154(18) 0.129(15) -0.004(14) 0.062(13) 0.052(13) O14B 0.040(12) 0.14(3) 0.09(2) 0.01(2) -0.009(13) 0.021(15) C1A 0.071(12) 0.048(9) 0.037(8) -0.012(6) -0.003(8) 0.001(9) C1B 0.128(16) 0.066(13) 0.062(15) 0.009(11) 0.014(15) 0.039(13) C11B 0.027(10) 0.035(10) 0.072(16) 0.033(11) -0.003(10) 0.004(8) C12B 0.051(15) 0.075(19) 0.050(15) 0.029(14) -0.020(12) 0.008(14) C15B 0.042(4) 0.035(3) 0.045(6) -0.006(4) -0.004(3) -0.008(4) C16B 0.043(4) 0.035(3) 0.045(6) -0.006(4) -0.004(3) -0.008(4) 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 O2 Mo1 Mo2 47.7(2) . . ? O2 Mo1 O11 68.1(3) . . ? O3 Mo1 Mo2 49.48(17) . . ? O3 Mo1 O2 97.1(3) . . ? O3 Mo1 O11 68.5(2) . . ? O7 Mo1 Mo2 128.6(2) . . ? O7 Mo1 O2 87.1(3) . . ? O7 Mo1 O3 153.0(3) . . ? O7 Mo1 O8 80.7(4) . . ? O7 Mo1 O11 88.8(3) . . ? O8 Mo1 Mo2 128.9(2) . . ? O8 Mo1 O2 155.6(4) . . ? O8 Mo1 O3 84.8(3) . . ? O8 Mo1 O11 90.4(3) . . ? O9 Mo1 Mo2 103.2(3) . . ? O9 Mo1 O2 97.7(4) . . ? O9 Mo1 O3 99.4(3) . . ? O9 Mo1 O7 106.5(4) . . ? O9 Mo1 O8 106.1(4) . . ? O9 Mo1 O11 158.9(3) . . ? O11 Mo1 Mo2 55.75(13) . . ? O2 Mo2 Mo1 49.6(2) . . ? O2 Mo2 O3 98.9(3) . . ? O2 Mo2 O11 70.3(3) . . ? O3 Mo2 Mo1 49.28(18) . . ? O3 Mo2 O11 69.7(2) . . ? O5 Mo2 Mo1 126.16(19) . . ? O5 Mo2 O2 149.7(3) . . ? O5 Mo2 O3 84.8(3) . . ? O5 Mo2 O11 83.2(2) . . ? O6 Mo2 Mo1 130.4(3) . . ? O6 Mo2 O2 85.6(3) . . ? O6 Mo2 O3 156.7(3) . . ? O6 Mo2 O5 80.2(3) . . ? O6 Mo2 O11 90.8(3) . . ? O10 Mo2 Mo1 102.4(3) . . ? O10 Mo2 O2 100.4(4) . . ? O10 Mo2 O3 95.2(3) . . ? O10 Mo2 O5 109.2(4) . . ? O10 Mo2 O6 106.4(4) . . ? O10 Mo2 O11 160.0(3) . . ? O11 Mo2 Mo1 57.97(16) . . ? O4 Mo3 Mo4 57.39(15) 1_554 . ? O12 Mo3 Mo4 47.79(18) . . ? O12 Mo3 O4 70.3(2) . 1_554 ? O13 Mo3 Mo4 48.83(18) . . ? O13 Mo3 O4 70.3(2) . 1_554 ? O13 Mo3 O12 96.5(3) . . ? O17 Mo3 Mo4 124.7(2) . . ? O17 Mo3 O4 83.7(3) . 1_554 ? O17 Mo3 O12 84.9(3) . . ? O17 Mo3 O13 151.6(3) . . ? O18 Mo3 Mo4 128.3(2) . . ? O18 Mo3 O4 86.7(2) . 1_554 ? O18 Mo3 O12 154.0(3) . . ? O18 Mo3 O13 86.6(3) . . ? O18 Mo3 O17 80.5(3) . . ? O19 Mo3 Mo4 106.5(3) . . ? O19 Mo3 O4 163.8(3) . 1_554 ? O19 Mo3 O12 97.7(4) . . ? O19 Mo3 O13 101.3(4) . . ? O19 Mo3 O17 106.6(4) . . ? O19 Mo3 O18 107.0(3) . . ? O4 Mo4 Mo3 55.99(13) 1_554 . ? O12 Mo4 Mo3 48.64(19) . . ? O12 Mo4 O4 69.8(2) . 1_554 ? O12 Mo4 O13 96.0(3) . . ? O13 Mo4 Mo3 47.4(2) . . ? O13 Mo4 O4 68.8(2) . 1_554 ? O15 Mo4 Mo3 127.4(2) . . ? O15 Mo4 O4 86.0(2) . 1_554 ? O15 Mo4 O12 152.0(3) . . ? O15 Mo4 O13 87.9(3) . . ? O16 Mo4 Mo3 125.89(17) . . ? O16 Mo4 O4 87.6(3) . 1_554 ? O16 Mo4 O12 83.9(3) . . ? O16 Mo4 O13 154.6(3) . . ? O16 Mo4 O15 81.1(3) . . ? O20 Mo4 Mo3 105.1(3) . . ? O20 Mo4 O4 161.1(3) . 1_554 ? O20 Mo4 O12 98.2(4) . . ? O20 Mo4 O13 99.1(3) . . ? O20 Mo4 O15 108.6(4) . . ? O20 Mo4 O16 106.0(3) . . ? Mo2 O2 Mo1 82.7(3) . . ? C2A O2 Mo1 144.1(15) . . ? C2A O2 Mo2 126.4(15) . . ? C1A O2 Mo1 137.7(10) . . ? C1A O2 Mo2 135.4(11) . . ? Mo1 O3 Mo2 81.2(2) . . ? C3 O3 Mo1 129.3(5) . . ? C3 O3 Mo2 129.8(5) . . ? Mo3 O4 Mo4 66.62(16) 1_556 1_556 ? C4 O4 Mo3 123.3(4) . 1_556 ? C4 O4 Mo4 121.9(5) . 1_556 ? Mo2 O5 H5 136(2) . . ? C5 O5 Mo2 114.9(6) . . ? C5 O5 H5 109(2) . . ? C6 O6 Mo2 114.2(7) . . ? C7 O7 Mo1 116.2(7) . . ? C8 O8 Mo1 113.4(7) . . ? Mo2 O11 Mo1 66.29(17) . . ? C9 O11 Mo1 121.0(6) . . ? C9 O11 Mo2 122.4(5) . . ? Mo4 O12 Mo3 83.6(3) . . ? C10 O12 Mo3 133.3(6) . . ? C10 O12 Mo4 129.7(5) . . ? Mo3 O13 Mo4 83.7(3) . . ? C11A O13 Mo3 134.6(11) . . ? C11A O13 Mo4 141.0(11) . . ? C11B O13 Mo3 132.0(13) . . ? C11B O13 Mo4 136.7(14) . . ? C13 O15 Mo4 116.1(5) . . ? C14 O16 Mo4 113.0(5) . . ? Mo3 O17 H17 131.4 . . ? Mo3 O17 H17A 130.3 . . ? C15A O17 Mo3 118.7(8) . . ? C15A O17 H17 109.5 . . ? C15B O17 Mo3 108.5(9) . . ? C15B O17 H17A 109.5 . . ? C16A O18 Mo3 110.6(9) . . ? C16B O18 Mo3 118.9(9) . . ? O3 C3 H3A 109.4 . . ? O3 C3 H3B 109.4 . . ? O3 C3 C4 111.3(7) . . ? H3A C3 H3B 108.0 . . ? C4 C3 H3A 109.4 . . ? C4 C3 H3B 109.4 . . ? O4 C4 C3 111.7(6) . . ? O4 C4 H4A 109.3 . . ? O4 C4 H4B 109.3 . . ? C3 C4 H4A 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 107.9 . . ? O5 C5 H5A 110.5 . . ? O5 C5 H5B 110.5 . . ? O5 C5 C6 106.0(9) . . ? H5A C5 H5B 108.7 . . ? C6 C5 H5A 110.5 . . ? C6 C5 H5B 110.5 . . ? O6 C6 C5 106.6(8) . . ? O6 C6 H6A 110.4 . . ? O6 C6 H6B 110.4 . . ? C5 C6 H6A 110.4 . . ? C5 C6 H6B 110.4 . . ? H6A C6 H6B 108.6 . . ? O7 C7 H7A 109.5 . . ? O7 C7 H7B 109.5 . . ? O7 C7 C8 110.5(10) . . ? H7A C7 H7B 108.1 . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? O8 C8 C7 108.5(10) . . ? O8 C8 H8A 110.0 . . ? O8 C8 H8B 110.0 . . ? C7 C8 H8A 110.0 . . ? C7 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? O11 C9 H9A 109.1 . . ? O11 C9 H9B 109.1 . . ? O11 C9 C10 112.3(8) . . ? H9A C9 H9B 107.9 . . ? C10 C9 H9A 109.1 . . ? C10 C9 H9B 109.1 . . ? O12 C10 C9 110.4(7) . . ? O12 C10 H10A 109.6 . . ? O12 C10 H10B 109.6 . . ? C9 C10 H10A 109.6 . . ? C9 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? O15 C13 H13A 110.1 . . ? O15 C13 H13B 110.1 . . ? O15 C13 C14 107.9(7) . . ? H13A C13 H13B 108.4 . . ? C14 C13 H13A 110.1 . . ? C14 C13 H13B 110.1 . . ? O16 C14 C13 106.9(7) . . ? O16 C14 H14A 110.3 . . ? O16 C14 H14B 110.3 . . ? C13 C14 H14A 110.3 . . ? C13 C14 H14B 110.3 . . ? H14A C14 H14B 108.6 . . ? C1 O1A H1A 109.5 . . ? C12A O14A H14C 109.5 . . ? O1A C1 H1B 109.7 . . ? O1A C1 H1C 109.7 . . ? O1A C1 C2A 110(3) . . ? H1B C1 H1C 108.2 . . ? C2A C1 H1B 109.7 . . ? C2A C1 H1C 109.7 . . ? O2 C2A H2AA 110.1 . . ? O2 C2A H2AB 110.1 . . ? C1 C2A O2 108(2) . . ? C1 C2A H2AA 110.1 . . ? C1 C2A H2AB 110.1 . . ? H2AA C2A H2AB 108.4 . . ? O13 C11A H11A 106.1 . . ? O13 C11A H11B 106.1 . . ? H11A C11A H11B 106.3 . . ? C12A C11A O13 125(2) . . ? C12A C11A H11A 106.1 . . ? C12A C11A H11B 106.1 . . ? O14A C12A C11A 132(2) . . ? O14A C12A H12A 104.4 . . ? O14A C12A H12B 104.4 . . ? C11A C12A H12A 104.4 . . ? C11A C12A H12B 104.4 . . ? H12A C12A H12B 105.6 . . ? O17 C15A H15A 112.0 . . ? O17 C15A H15B 112.0 . . ? O17 C15A C16A 98.9(12) . . ? H15A C15A H15B 109.7 . . ? C16A C15A H15A 112.0 . . ? C16A C15A H15B 112.0 . . ? O18 C16A C15A 109.7(11) . . ? O18 C16A H16A 109.7 . . ? O18 C16A H16B 109.7 . . ? C15A C16A H16A 109.7 . . ? C15A C16A H16B 109.7 . . ? H16A C16A H16B 108.2 . . ? C1B O1B H1BA 109.5 . . ? C12B O14B H14D 109.5 . . ? O2 C1A H1AA 110.7 . . ? O2 C1A H1AB 110.7 . . ? H1AA C1A H1AB 108.8 . . ? C1B C1A O2 105.4(18) . . ? C1B C1A H1AA 110.7 . . ? C1B C1A H1AB 110.7 . . ? O1B C1B C1A 106(3) . . ? O1B C1B H1BB 110.6 . . ? O1B C1B H1BC 110.6 . . ? C1A C1B H1BB 110.6 . . ? C1A C1B H1BC 110.6 . . ? H1BB C1B H1BC 108.7 . . ? O13 C11B H11C 111.1 . . ? O13 C11B H11D 111.1 . . ? H11C C11B H11D 109.1 . . ? C12B C11B O13 103(2) . . ? C12B C11B H11C 111.1 . . ? C12B C11B H11D 111.1 . . ? O14B C12B C11B 117(3) . . ? O14B C12B H12C 108.1 . . ? O14B C12B H12D 108.1 . . ? C11B C12B H12C 108.1 . . ? C11B C12B H12D 108.1 . . ? H12C C12B H12D 107.3 . . ? O17 C15B H15C 110.3 . . ? O17 C15B H15D 110.3 . . ? H15C C15B H15D 108.5 . . ? C16B C15B O17 107.3(14) . . ? C16B C15B H15C 110.3 . . ? C16B C15B H15D 110.3 . . ? O18 C16B C15B 105.7(15) . . ? O18 C16B H16C 110.6 . . ? O18 C16B H16D 110.6 . . ? C15B C16B H16C 110.6 . . ? C15B C16B H16D 110.6 . . ? H16C C16B H16D 108.7 . . ? 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 2.6786(10) . ? Mo1 O2 2.057(7) . ? Mo1 O3 2.054(6) . ? Mo1 O7 1.921(8) . ? Mo1 O8 1.937(7) . ? Mo1 O9 1.667(8) . ? Mo1 O11 2.480(7) . ? Mo2 O2 1.996(8) . ? Mo2 O3 2.060(6) . ? Mo2 O5 1.961(6) . ? Mo2 O6 1.920(7) . ? Mo2 O10 1.675(8) . ? Mo2 O11 2.418(6) . ? Mo3 Mo4 2.7030(10) . ? Mo3 O4 2.441(6) 1_554 ? Mo3 O12 2.042(7) . ? Mo3 O13 2.003(8) . ? Mo3 O17 1.957(8) . ? Mo3 O18 1.923(7) . ? Mo3 O19 1.683(8) . ? Mo4 O4 2.481(6) 1_554 ? Mo4 O12 2.015(7) . ? Mo4 O13 2.047(6) . ? Mo4 O15 1.936(7) . ? Mo4 O16 1.922(6) . ? Mo4 O20 1.675(8) . ? O2 C2A 1.49(2) . ? O2 C1A 1.49(2) . ? O3 C3 1.424(11) . ? O4 C4 1.446(9) . ? O5 H5 0.873(13) . ? O5 C5 1.447(11) . ? O6 C6 1.417(13) . ? O7 C7 1.414(12) . ? O8 C8 1.401(15) . ? O11 C9 1.438(11) . ? O12 C10 1.477(12) . ? O13 C11A 1.43(2) . ? O13 C11B 1.41(2) . ? O15 C13 1.430(11) . ? O16 C14 1.418(11) . ? O17 H17 0.8400 . ? O17 H17A 0.8400 . ? O17 C15A 1.465(16) . ? O17 C15B 1.497(17) . ? O18 C16A 1.449(15) . ? O18 C16B 1.408(18) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.500(12) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5 C6 1.478(16) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.49(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9 C10 1.480(13) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 C14 1.510(14) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? O1A H1A 0.8400 . ? O1A C1 1.42(3) . ? O14A H14C 0.8400 . ? O14A C12A 1.35(2) . ? C1 H1B 0.9900 . ? C1 H1C 0.9900 . ? C1 C2A 1.47(3) . ? C2A H2AA 0.9900 . ? C2A H2AB 0.9900 . ? C11A H11A 0.9900 . ? C11A H11B 0.9900 . ? C11A C12A 1.38(2) . ? C12A H12A 0.9900 . ? C12A H12B 0.9900 . ? C15A H15A 0.9900 . ? C15A H15B 0.9900 . ? C15A C16A 1.521(19) . ? C16A H16A 0.9900 . ? C16A H16B 0.9900 . ? O1B H1BA 0.8400 . ? O1B C1B 1.43(4) . ? O14B H14D 0.8400 . ? O14B C12B 1.38(3) . ? C1A H1AA 0.9900 . ? C1A H1AB 0.9900 . ? C1A C1B 1.49(3) . ? C1B H1BB 0.9900 . ? C1B H1BC 0.9900 . ? C11B H11C 0.9900 . ? C11B H11D 0.9900 . ? C11B C12B 1.39(3) . ? C12B H12C 0.9900 . ? C12B H12D 0.9900 . ? C15B H15C 0.9900 . ? C15B H15D 0.9900 . ? C15B C16B 1.46(2) . ? C16B H16C 0.9900 . ? C16B H16D 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 O5 H5 O4 0.873(13) 1.83(3) 2.582(9) 142(3) . yes O5 H5 O18 0.873(13) 2.67(6) 3.273(9) 127(6) 1_556 yes O17 H17 O11 0.84 1.79 2.561(10) 151.7 . yes C5 H5B O18 0.99 2.52 3.268(15) 132.6 1_556 yes C6 H6B O14B 0.99 2.32 3.19(4) 147.0 2_675 yes C8 H8A O1A 0.99 2.08 2.91(4) 140.2 3_545 yes C13 H13A O10 0.99 2.52 3.203(12) 126.1 1_544 yes C14 H14B O10 0.99 2.42 3.066(12) 122.5 1_544 yes O1A H1A O7 0.84 2.23 2.67(4) 112.9 . yes O14A H14C O15 0.84 1.86 2.685(13) 168.7 . 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 O2 C2A C1 -33(4) . . . . ? Mo1 O2 C1A C1B 116(2) . . . . ? Mo1 O3 C3 C4 -161.7(5) . . . . ? Mo1 O7 C7 C8 4.0(15) . . . . ? Mo1 O8 C8 C7 36.1(17) . . . . ? Mo1 O11 C9 C10 82.6(9) . . . . ? Mo2 O2 C2A C1 -171.3(16) . . . . ? Mo2 O2 C1A C1B -96(2) . . . . ? Mo2 O3 C3 C4 -46.6(10) . . . . ? Mo2 O5 C5 C6 28.2(10) . . . . ? Mo2 O6 C6 C5 42.9(11) . . . . ? Mo2 O11 C9 C10 162.6(6) . . . . ? Mo3 O4 C4 C3 -165.0(6) 1_556 . . . ? Mo3 O12 C10 C9 41.3(13) . . . . ? Mo3 O13 C11A C12A -176(3) . . . . ? Mo3 O13 C11B C12B 129.5(17) . . . . ? Mo3 O17 C15A C16A -31.1(14) . . . . ? Mo3 O17 C15B C16B 45.8(18) . . . . ? Mo3 O18 C16A C15A -47.0(16) . . . . ? Mo3 O18 C16B C15B 23(2) . . . . ? Mo4 O4 C4 C3 -83.6(8) 1_556 . . . ? Mo4 O12 C10 C9 167.0(7) . . . . ? Mo4 O13 C11A C12A 17(5) . . . . ? Mo4 O13 C11B C12B -93(2) . . . . ? Mo4 O15 C13 C14 -16.0(10) . . . . ? Mo4 O16 C14 C13 -42.1(10) . . . . ? O2 C1A C1B O1B -60(3) . . . . ? O3 C3 C4 O4 -56.3(10) . . . . ? O5 C5 C6 O6 -43.5(12) . . . . ? O7 C7 C8 O8 -25.2(18) . . . . ? O11 C9 C10 O12 58.6(12) . . . . ? O13 C11A C12A O14A 36(6) . . . . ? O13 C11B C12B O14B -80(3) . . . . ? O15 C13 C14 O16 35.9(11) . . . . ? O17 C15A C16A O18 47.4(17) . . . . ? O17 C15B C16B O18 -43(2) . . . . ? O1A C1 C2A O2 -61(3) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.95(8) 2 0.05(8)