Electrochemical and X-ray structural evidence of multiple molybdenum precursor candidates from a reported non-aqueous electrodeposition of molybdenum disulfide
George, Tanner; Brosseau, Christa L.; Masuda, Jason D.; RSC Advances 13 (2023) 32199–32216; doi:10.1039/D3RA04605B

data_7247664
_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_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_checksum              84872
_olex2_submission_special_instructions 'No special instructions were received'