#------------------------------------------------------------------------------ #$Date: 2023-11-02 04:30:41 +0200 (Thu, 02 Nov 2023) $ #$Revision: 287242 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/76/7247663.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_7247663 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 'C4 H10 Mo O6' _chemical_formula_sum 'C4 H10 Mo O6' _chemical_formula_weight 250.06 _space_group_crystal_system tetragonal _space_group_IT_number 76 _space_group_name_Hall 'P 4w' _space_group_name_H-M_alt 'P 41' _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 8 _cell_length_a 9.46450(10) _cell_length_b 9.46450(10) _cell_length_c 17.3160(4) _cell_measurement_reflns_used 9030 _cell_measurement_temperature 100.0 _cell_measurement_theta_max 52.15 _cell_measurement_theta_min 2.45 _cell_volume 1551.11(4) _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 100.00 _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 0.993 _diffrn_measured_fraction_theta_max 0.998 _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 0.0334 _diffrn_reflns_av_unetI/netI 0.0174 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_number 110585 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 44.998 _diffrn_reflns_theta_min 2.152 _diffrn_source 'microfocus sealed tube' _diffrn_source_type 'Incoatec I\mS 3.0' _exptl_absorpt_coefficient_mu 1.675 _exptl_absorpt_correction_T_max 0.7503 _exptl_absorpt_correction_T_min 0.6410 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0996 before and 0.0613 after correction. The Ratio of minimum to maximum transmission is 0.8543. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 2.142 _exptl_crystal_description prism _exptl_crystal_F_000 992 _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.265 _exptl_crystal_size_min 0.225 _refine_diff_density_max 1.026 _refine_diff_density_min -1.376 _refine_diff_density_rms 0.099 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.03(2) _refine_ls_extinction_coef 0.0023(4) _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 1.101 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 214 _refine_ls_number_reflns 12760 _refine_ls_number_restraints 4 _refine_ls_restrained_S_all 1.101 _refine_ls_R_factor_all 0.0223 _refine_ls_R_factor_gt 0.0208 _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^)+(0.0163P)^2^+1.0349P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.0518 _reflns_Friedel_coverage 0.957 _reflns_Friedel_fraction_full 0.990 _reflns_Friedel_fraction_max 0.998 _reflns_number_gt 12338 _reflns_number_total 12760 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ra04605b2.cif _cod_data_source_block mo_2019_09_24_jdm_tg_moglyc_0m_a _cod_original_cell_volume 1551.11(5) _cod_database_code 7247663 _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. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.97(2) 0.03(2) 2. Fixed Uiso At 1.2 times of: All C(H,H) groups At 1.5 times of: All O(H) groups 3. Restrained distances O6-H6 0.87 with sigma of 0.01 O10-H10 0.87 with sigma of 0.01 O4-H4 0.87 with sigma of 0.01 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) ; _shelx_res_file ; TITL mo_2019_09_24_JDM_TG_MoGlyc_0m_a.res in P4(1) mo_2019_09_24_jdm_tg_moglyc_0m_a.res created by SHELXL-2018/3 at 21:03:09 on 10-Sep-2023 REM Old TITL mo_2019_09_24_JDM_TG_MoGlyc_0m in P4/m REM SHELXT solution in P4(1): R1 0.167, Rweak 0.012, Alpha 0.116 REM 12.604 for 15 systematic absences, Orientation as input REM Flack x = 0.246 ( 0.013 ) from 1514 Parsons' quotients REM Formula found by SHELXT: C13 Mo2 O10 CELL 0.71073 9.4645 9.4645 17.316 90 90 90 ZERR 8 0.0001 0.0001 0.0004 0 0 0 LATT -1 SYMM -X,-Y,0.5+Z SYMM -Y,+X,0.25+Z SYMM +Y,-X,0.75+Z SFAC C H Mo O UNIT 32 80 8 48 EQIV $1 +Y,2-X,-0.25+Z EQIV $2 1+Y,2-X,-0.25+Z EQIV $3 2-X,1-Y,0.5+Z DFIX 0.87 0.01 O6 H6 DFIX 0.87 0.01 O10 H10 DFIX 0.87 0.01 O4 H4 L.S. 10 PLAN 5 TEMP -173.15 CONF HTAB O6 O9 HTAB O12 O11_$1 HTAB O4 O3_$2 HTAB O10 O5_$3 LIST 4 MORE -1 BOND $H fmap 2 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 OMIT -3 90 REM REM REM WGHT 0.016300 1.034900 EXTI 0.002314 BASF 0.02791 FVAR 0.51462 MO1 3 1.253206 0.312624 0.248545 11.00000 0.00993 0.00817 = 0.00852 0.00044 0.00019 0.00040 O1 4 1.350084 0.272923 0.168502 11.00000 0.01800 0.01558 = 0.01431 0.00020 0.00506 0.00297 O2 4 1.233142 0.156631 0.296360 11.00000 0.01742 0.01098 = 0.01488 0.00358 0.00063 -0.00045 O3 4 1.395228 0.387200 0.320733 11.00000 0.01192 0.01403 = 0.01471 0.00145 -0.00284 -0.00193 O4 4 1.283042 0.547378 0.212463 11.00000 0.01475 0.01172 = 0.01257 0.00151 0.00039 -0.00118 H4 2 1.315806 0.559482 0.167162 11.00000 -1.50000 O5 4 1.071922 0.328333 0.194163 11.00000 0.01235 0.01270 = 0.00939 -0.00204 -0.00125 0.00072 O6 4 1.106180 0.427969 0.330201 11.00000 0.01102 0.01580 = 0.01127 -0.00501 -0.00041 0.00131 H6 2 1.132748 0.482330 0.366758 11.00000 -1.50000 C1 1 1.475024 0.509475 0.299293 11.00000 0.01503 0.02026 = 0.02119 0.00462 -0.00370 -0.00605 AFIX 23 H1A 2 1.546598 0.484033 0.259988 11.00000 -1.20000 H1B 2 1.524535 0.548308 0.344964 11.00000 -1.20000 AFIX 0 C2 1 1.373981 0.618298 0.266866 11.00000 0.02195 0.01271 = 0.01729 0.00063 -0.00207 -0.00434 AFIX 23 H2A 2 1.317191 0.660581 0.308950 11.00000 -1.20000 H2B 2 1.427157 0.694669 0.240760 11.00000 -1.20000 AFIX 0 C3 1 0.944958 0.357268 0.237203 11.00000 0.01166 0.01533 = 0.01333 -0.00205 -0.00076 -0.00120 AFIX 23 H3A 2 0.914092 0.271597 0.265335 11.00000 -1.20000 H3B 2 0.868193 0.386505 0.201807 11.00000 -1.20000 AFIX 0 C4 1 0.977496 0.473722 0.293108 11.00000 0.01189 0.01402 = 0.01422 -0.00268 0.00003 0.00187 AFIX 23 H4A 2 0.991731 0.564528 0.265817 11.00000 -1.20000 H4B 2 0.900340 0.484967 0.331219 11.00000 -1.20000 AFIX 0 MO02 3 1.192450 0.763953 0.497094 11.00000 0.00845 0.00988 = 0.00716 -0.00191 -0.00039 -0.00003 O7 4 1.338500 0.764120 0.439882 11.00000 0.01209 0.01863 = 0.01525 -0.00459 0.00375 -0.00093 O8 4 1.248924 0.711440 0.585941 11.00000 0.01564 0.01637 = 0.01123 0.00051 -0.00316 0.00111 O9 4 1.113275 0.588656 0.454805 11.00000 0.01253 0.01194 = 0.01201 -0.00324 0.00088 -0.00178 O10 4 0.961083 0.749321 0.548139 11.00000 0.01112 0.01334 = 0.00956 -0.00076 0.00091 -0.00100 H10 2 0.951871 0.736145 0.596748 11.00000 0.02158 O11 4 1.181193 0.965068 0.528124 11.00000 0.01319 0.01113 = 0.00830 -0.00157 -0.00055 -0.00057 O12 4 1.057037 0.869850 0.410854 11.00000 0.01884 0.01317 = 0.00945 -0.00100 -0.00516 0.00137 H12 2 1.025554 0.847530 0.372502 11.00000 -1.50000 C5 1 1.001306 0.521137 0.496632 11.00000 0.01572 0.01299 = 0.01405 -0.00137 0.00136 -0.00334 AFIX 23 H5A 2 1.037349 0.482291 0.545925 11.00000 -1.20000 H5B 2 0.961130 0.442665 0.465861 11.00000 -1.20000 AFIX 0 C6 1 0.889737 0.631771 0.512004 11.00000 0.01112 0.01709 = 0.01352 -0.00190 0.00044 -0.00313 AFIX 23 H6A 2 0.844859 0.661963 0.463068 11.00000 -1.20000 H6B 2 0.815696 0.593696 0.546614 11.00000 -1.20000 AFIX 0 C7 1 1.147894 1.069886 0.471346 11.00000 0.01502 0.01242 = 0.01287 0.00136 -0.00223 -0.00179 AFIX 23 H7A 2 1.229661 1.085621 0.436743 11.00000 -1.20000 H7B 2 1.123620 1.160513 0.496625 11.00000 -1.20000 AFIX 0 C8 1 1.023661 1.014992 0.426134 11.00000 0.01309 0.01348 = 0.01320 -0.00010 -0.00187 0.00089 AFIX 23 H8A 2 0.935527 1.022758 0.456632 11.00000 -1.20000 H8B 2 1.011994 1.068279 0.377351 11.00000 -1.20000 AFIX 0 HKLF 4 REM mo_2019_09_24_JDM_TG_MoGlyc_0m_a.res in P4(1) REM wR2 = 0.0518, GooF = S = 1.101, Restrained GooF = 1.101 for all data REM R1 = 0.0208 for 12338 Fo > 4sig(Fo) and 0.0223 for all 12760 data REM 214 parameters refined using 4 restraints END WGHT 0.0167 1.0044 REM Highest difference peak 1.026, deepest hole -1.376, 1-sigma level 0.099 Q1 1 1.1829 0.8039 0.4816 11.00000 0.05 1.03 Q2 1 1.2198 0.3406 0.2698 11.00000 0.05 0.85 Q3 1 1.1789 0.7960 0.5169 11.00000 0.05 0.79 Q4 1 1.2291 0.3304 0.2261 11.00000 0.05 0.79 Q5 1 1.2390 0.7613 0.5100 11.00000 0.05 0.77 ; _shelx_res_checksum 93760 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+1/4' 'y, -x, z+3/4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 1.25321(2) 0.31262(2) 0.24855(2) 0.00887(2) Uani 1 1 d . . . . . O1 O 1.35008(16) 0.27292(15) 0.16850(8) 0.0160(2) Uani 1 1 d . . . . . O2 O 1.23314(15) 0.15663(14) 0.29636(8) 0.01443(19) Uani 1 1 d . . . . . O3 O 1.39523(14) 0.38720(14) 0.32073(8) 0.01355(18) Uani 1 1 d . . . . . O4 O 1.28304(14) 0.54738(13) 0.21246(7) 0.01301(18) Uani 1 1 d D . . . . H4 H 1.316(4) 0.559(4) 0.1672(11) 0.020 Uiso 1 1 d D U . . . O5 O 1.07192(13) 0.32833(13) 0.19416(7) 0.01148(16) Uani 1 1 d . . . . . O6 O 1.10618(13) 0.42797(14) 0.33020(7) 0.01270(18) Uani 1 1 d D . . . . H6 H 1.133(4) 0.482(3) 0.3668(16) 0.019 Uiso 1 1 d D U . . . C1 C 1.4750(2) 0.5095(2) 0.29929(12) 0.0188(3) Uani 1 1 d . . . . . H1A H 1.546598 0.484033 0.259988 0.023 Uiso 1 1 calc R U . . . H1B H 1.524535 0.548308 0.344964 0.023 Uiso 1 1 calc R U . . . C2 C 1.3740(2) 0.61830(19) 0.26687(11) 0.0173(3) Uani 1 1 d . . . . . H2A H 1.317191 0.660581 0.308950 0.021 Uiso 1 1 calc R U . . . H2B H 1.427157 0.694669 0.240760 0.021 Uiso 1 1 calc R U . . . C3 C 0.94496(17) 0.35727(18) 0.23720(9) 0.0134(2) Uani 1 1 d . . . . . H3A H 0.914092 0.271597 0.265335 0.016 Uiso 1 1 calc R U . . . H3B H 0.868193 0.386505 0.201807 0.016 Uiso 1 1 calc R U . . . C4 C 0.97750(17) 0.47372(18) 0.29311(10) 0.0134(2) Uani 1 1 d . . . . . H4A H 0.991731 0.564528 0.265817 0.016 Uiso 1 1 calc R U . . . H4B H 0.900340 0.484967 0.331219 0.016 Uiso 1 1 calc R U . . . Mo02 Mo 1.19245(2) 0.76395(2) 0.49709(2) 0.00850(2) Uani 1 1 d . . . . . O7 O 1.33850(14) 0.76412(15) 0.43988(8) 0.0153(2) Uani 1 1 d . . . . . O8 O 1.24892(14) 0.71144(15) 0.58594(8) 0.01441(19) Uani 1 1 d . . . . . O9 O 1.11328(13) 0.58866(13) 0.45481(7) 0.01216(17) Uani 1 1 d . . . . . O10 O 0.96108(13) 0.74932(13) 0.54814(7) 0.01134(16) Uani 1 1 d D . . . . H10 H 0.952(4) 0.736(4) 0.5967(9) 0.022(9) Uiso 1 1 d D . . . . O11 O 1.18119(13) 0.96507(13) 0.52812(7) 0.01087(16) Uani 1 1 d . . . . . O12 O 1.05704(15) 0.86985(14) 0.41085(7) 0.01382(19) Uani 1 1 d . . . . . H12 H 1.026(4) 0.848(4) 0.373(2) 0.021 Uiso 1 1 d . U . . . C5 C 1.00131(18) 0.52114(15) 0.49663(12) 0.0143(2) Uani 1 1 d . . . . . H5A H 1.037349 0.482291 0.545925 0.017 Uiso 1 1 calc R U . . . H5B H 0.961130 0.442665 0.465861 0.017 Uiso 1 1 calc R U . . . C6 C 0.88974(17) 0.63177(19) 0.51200(9) 0.0139(2) Uani 1 1 d . . . . . H6A H 0.844859 0.661963 0.463068 0.017 Uiso 1 1 calc R U . . . H6B H 0.815696 0.593696 0.546614 0.017 Uiso 1 1 calc R U . . . C7 C 1.14789(18) 1.06989(18) 0.47135(10) 0.0134(2) Uani 1 1 d . . . . . H7A H 1.229661 1.085621 0.436743 0.016 Uiso 1 1 calc R U . . . H7B H 1.123620 1.160513 0.496625 0.016 Uiso 1 1 calc R U . . . C8 C 1.02366(18) 1.01499(18) 0.42613(10) 0.0133(2) Uani 1 1 d . . . . . H8A H 0.935527 1.022758 0.456632 0.016 Uiso 1 1 calc R U . . . H8B H 1.011994 1.068279 0.377351 0.016 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 0.00993(4) 0.00817(4) 0.00852(4) 0.00044(4) 0.00019(4) 0.00040(3) O1 0.0180(5) 0.0156(5) 0.0143(5) 0.0002(4) 0.0051(4) 0.0030(4) O2 0.0174(5) 0.0110(4) 0.0149(5) 0.0036(4) 0.0006(4) -0.0004(4) O3 0.0119(4) 0.0140(4) 0.0147(4) 0.0015(3) -0.0028(3) -0.0019(3) O4 0.0147(5) 0.0117(4) 0.0126(4) 0.0015(3) 0.0004(3) -0.0012(3) O5 0.0123(4) 0.0127(4) 0.0094(4) -0.0020(3) -0.0013(3) 0.0007(3) O6 0.0110(4) 0.0158(5) 0.0113(4) -0.0050(3) -0.0004(3) 0.0013(3) C1 0.0150(6) 0.0203(7) 0.0212(7) 0.0046(6) -0.0037(5) -0.0061(5) C2 0.0220(7) 0.0127(6) 0.0173(6) 0.0006(5) -0.0021(5) -0.0043(5) C3 0.0117(5) 0.0153(5) 0.0133(6) -0.0021(4) -0.0008(4) -0.0012(4) C4 0.0119(5) 0.0140(5) 0.0142(5) -0.0027(4) 0.0000(4) 0.0019(4) Mo02 0.00845(4) 0.00988(4) 0.00716(4) -0.00191(4) -0.00039(3) -0.00003(3) O7 0.0121(4) 0.0186(5) 0.0153(5) -0.0046(4) 0.0038(4) -0.0009(4) O8 0.0156(5) 0.0164(5) 0.0112(4) 0.0005(4) -0.0032(3) 0.0011(4) O9 0.0125(4) 0.0119(4) 0.0120(4) -0.0032(3) 0.0009(3) -0.0018(3) O10 0.0111(4) 0.0133(4) 0.0096(4) -0.0008(3) 0.0009(3) -0.0010(3) O11 0.0132(4) 0.0111(4) 0.0083(3) -0.0016(3) -0.0005(3) -0.0006(3) O12 0.0188(5) 0.0132(4) 0.0094(4) -0.0010(3) -0.0052(4) 0.0014(4) C5 0.0157(5) 0.0130(5) 0.0141(5) -0.0014(6) 0.0014(5) -0.0033(4) C6 0.0111(5) 0.0171(6) 0.0135(6) -0.0019(4) 0.0004(4) -0.0031(4) C7 0.0150(6) 0.0124(5) 0.0129(5) 0.0014(4) -0.0022(4) -0.0018(4) C8 0.0131(5) 0.0135(5) 0.0132(5) -0.0001(4) -0.0019(4) 0.0009(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 O1 Mo1 O3 103.20(7) . . ? O1 Mo1 O4 85.80(6) . . ? O1 Mo1 O5 95.56(7) . . ? O1 Mo1 O6 160.91(6) . . ? O2 Mo1 O1 105.32(7) . . ? O2 Mo1 O3 94.49(6) . . ? O2 Mo1 O4 166.50(6) . . ? O2 Mo1 O5 101.62(6) . . ? O2 Mo1 O6 92.63(6) . . ? O3 Mo1 O4 75.22(5) . . ? O3 Mo1 O6 81.38(5) . . ? O5 Mo1 O3 151.07(5) . . ? O5 Mo1 O4 84.54(5) . . ? O5 Mo1 O6 74.09(5) . . ? O6 Mo1 O4 77.39(5) . . ? C1 O3 Mo1 119.08(11) . . ? Mo1 O4 H4 115(2) . . ? C2 O4 Mo1 109.99(10) . . ? C2 O4 H4 109(2) . . ? C3 O5 Mo1 119.70(10) . . ? Mo1 O6 H6 125(2) . . ? C4 O6 Mo1 112.66(9) . . ? C4 O6 H6 113(2) . . ? O3 C1 H1A 110.0 . . ? O3 C1 H1B 110.0 . . ? O3 C1 C2 108.25(15) . . ? H1A C1 H1B 108.4 . . ? C2 C1 H1A 110.0 . . ? C2 C1 H1B 110.0 . . ? O4 C2 C1 107.63(15) . . ? O4 C2 H2A 110.2 . . ? O4 C2 H2B 110.2 . . ? C1 C2 H2A 110.2 . . ? C1 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? O5 C3 H3A 110.2 . . ? O5 C3 H3B 110.2 . . ? O5 C3 C4 107.61(13) . . ? H3A C3 H3B 108.5 . . ? C4 C3 H3A 110.2 . . ? C4 C3 H3B 110.2 . . ? O6 C4 C3 103.90(13) . . ? O6 C4 H4A 111.0 . . ? O6 C4 H4B 111.0 . . ? C3 C4 H4A 111.0 . . ? C3 C4 H4B 111.0 . . ? H4A C4 H4B 109.0 . . ? O7 Mo02 O8 105.75(7) . . ? O7 Mo02 O9 95.38(6) . . ? O7 Mo02 O10 165.97(6) . . ? O7 Mo02 O11 101.59(6) . . ? O7 Mo02 O12 94.44(6) . . ? O8 Mo02 O9 102.14(6) . . ? O8 Mo02 O10 86.32(6) . . ? O8 Mo02 O11 93.00(6) . . ? O8 Mo02 O12 157.75(6) . . ? O9 Mo02 O10 74.72(5) . . ? O9 Mo02 O11 153.28(5) . . ? O9 Mo02 O12 84.82(5) . . ? O11 Mo02 O10 84.55(5) . . ? O11 Mo02 O12 73.51(5) . . ? O12 Mo02 O10 75.05(5) . . ? C5 O9 Mo02 118.07(10) . . ? Mo02 O10 H10 118(3) . . ? C6 O10 Mo02 108.43(9) . . ? C6 O10 H10 105(3) . . ? C7 O11 Mo02 119.43(10) . . ? Mo02 O12 H12 134(3) . . ? C8 O12 Mo02 115.96(9) . . ? C8 O12 H12 110(3) . . ? O9 C5 H5A 110.3 . . ? O9 C5 H5B 110.3 . . ? O9 C5 C6 107.26(13) . . ? H5A C5 H5B 108.5 . . ? C6 C5 H5A 110.3 . . ? C6 C5 H5B 110.3 . . ? O10 C6 C5 106.47(13) . . ? O10 C6 H6A 110.4 . . ? O10 C6 H6B 110.4 . . ? C5 C6 H6A 110.4 . . ? C5 C6 H6B 110.4 . . ? H6A C6 H6B 108.6 . . ? O11 C7 H7A 110.4 . . ? O11 C7 H7B 110.4 . . ? O11 C7 C8 106.86(13) . . ? H7A C7 H7B 108.6 . . ? C8 C7 H7A 110.4 . . ? C8 C7 H7B 110.4 . . ? O12 C8 C7 104.75(13) . . ? O12 C8 H8A 110.8 . . ? O12 C8 H8B 110.8 . . ? C7 C8 H8A 110.8 . . ? C7 C8 H8B 110.8 . . ? H8A C8 H8B 108.9 . . ? 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 O1 1.7038(14) . ? Mo1 O2 1.7033(13) . ? Mo1 O3 1.9666(13) . ? Mo1 O4 2.3252(13) . ? Mo1 O5 1.9628(12) . ? Mo1 O6 2.2644(12) . ? O3 C1 1.431(2) . ? O4 H4 0.851(13) . ? O4 C2 1.442(2) . ? O5 C3 1.440(2) . ? O6 H6 0.854(13) . ? O6 C4 1.443(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C1 C2 1.513(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.499(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? Mo02 O7 1.7006(13) . ? Mo02 O8 1.7028(13) . ? Mo02 O9 1.9622(12) . ? Mo02 O10 2.3655(12) . ? Mo02 O11 1.9807(12) . ? Mo02 O12 2.2084(13) . ? O9 C5 1.434(2) . ? O10 H10 0.855(13) . ? O10 C6 1.444(2) . ? O11 C7 1.432(2) . ? O12 H12 0.76(4) . ? O12 C8 1.434(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5 C6 1.511(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.505(2) . ? C8 H8A 0.9900 . ? C8 H8B 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 O4 H4 O3 0.851(13) 1.852(14) 2.7000(18) 174(4) 4_674 yes O6 H6 O9 0.854(13) 1.836(19) 2.6406(17) 156(4) . yes O10 H10 O5 0.855(13) 1.808(15) 2.6517(16) 169(4) 2_765 yes O12 H12 O11 0.76(4) 1.75(4) 2.5047(17) 171(4) 4_574 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 46.1(2) . . . . ? Mo1 O4 C2 C1 29.87(17) . . . . ? Mo1 O5 C3 C4 45.17(16) . . . . ? Mo1 O6 C4 C3 36.07(15) . . . . ? O3 C1 C2 O4 -47.0(2) . . . . ? O5 C3 C4 O6 -49.29(16) . . . . ? Mo02 O9 C5 C6 51.51(17) . . . . ? Mo02 O10 C6 C5 33.13(14) . . . . ? Mo02 O11 C7 C8 46.54(16) . . . . ? Mo02 O12 C8 C7 29.08(16) . . . . ? O9 C5 C6 O10 -52.76(17) . . . . ? O11 C7 C8 O12 -44.58(17) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.97(2) 2 0.03(2)