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_7247660
_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         'C12 H26 Mo2 O11'
_chemical_formula_sum            'C12 H26 Mo2 O11'
_chemical_formula_weight         538.21
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_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                   16.7363(3)
_cell_length_b                   24.6210(5)
_cell_length_c                   8.8062(2)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    125.0
_cell_measurement_theta_max      45.19
_cell_measurement_theta_min      2.74
_cell_volume                     3628.72(13)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      125.00
_diffrn_detector_area_resol_mean 7.3910
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '\k--geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            39690
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         45.291
_diffrn_reflns_theta_min         2.741
_exptl_absorpt_coefficient_mu    1.436
_exptl_absorpt_correction_T_max  0.7494
_exptl_absorpt_correction_T_min  0.7016
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0940 before and 0.0584 after correction. The Ratio of minimum to maximum transmission is 0.9362. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.970
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.115
_refine_diff_density_max         0.836
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details
;
 Flack x determined using 2123 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.015(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         7050
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0160P)^2^+1.3443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0448
_refine_ls_wR_factor_ref         0.0487
_reflns_Friedel_coverage         0.782
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.851
_reflns_number_gt                5824
_reflns_number_total             7050
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ra04605b2.cif
_cod_data_source_block           mo_2020_1_6_jdm_tg89_0ma_a
_cod_database_code               7247660
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.852
_shelx_estimated_absorpt_t_min   0.803
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.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)
;
_shelx_res_checksum              56422
_olex2_submission_special_instructions 'No special instructions were received'