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_7247661
_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         'Mo6 O19, 2(C9 H20 N)'
_chemical_formula_sum            'C18 H40 Mo6 N2 O19'
_chemical_formula_weight         1164.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_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                 101.838(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.4347(8)
_cell_length_b                   16.0288(12)
_cell_length_c                   10.9136(9)
_cell_measurement_reflns_used    9194
_cell_measurement_temperature    125.0
_cell_measurement_theta_max      33.18
_cell_measurement_theta_min      2.29
_cell_volume                     1615.3(2)
_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 1.000
_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  0.0377
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            55716
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.259
_diffrn_reflns_theta_min         2.291
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS 3.0'
_exptl_absorpt_coefficient_mu    2.339
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.5705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0832 before and 0.0581 after correction. The Ratio of minimum to maximum transmission is 0.7642. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.393
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.772
_refine_diff_density_min         -1.142
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         6194
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.211
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0332
_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^)+6.6219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0731
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5542
_reflns_number_total             6194
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ra04605b2.cif
_cod_data_source_block           mo_2020_09_16_jdm_tg187wash2_0_a
_cod_database_code               7247661
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.853
_shelx_estimated_absorpt_t_min   0.665
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1A-C1A \\sim N1B-C1B
 with sigma of 0.02
 N1A-C2A \\sim N1B-C2B
 with sigma of 0.02
 N1A-C5 \\sim N1B-C5
 with sigma of 0.02
 N1A-C9 \\sim N1B-C9
 with sigma of 0.02
 C2A-C3A \\sim C2B-C3B
 with sigma of 0.02
 C3A-C4A \\sim C3B-C4B
 with sigma of 0.02
 N1A-C3A \\sim N1B-C3B
 with sigma of 0.04
 C1A-C2A \\sim C1B-C2B
 with sigma of 0.04
 C1A-C5 \\sim C1B-C5
 with sigma of 0.04
 C1A-C9 \\sim C1B-C9
 with sigma of 0.04
 C2A-C4A \\sim C2B-C4B
 with sigma of 0.04
 C2A-C5 \\sim C2B-C5
 with sigma of 0.04
 C2A-C9 \\sim C2B-C9
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 N1A, C1A, C2A, C3A, C4A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1B, C1B, C2B, C3B, C4B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H5BC)=Sof(H5BD)=Sof(H9BC)=Sof(H9BD)=Sof(C1B)=Sof(H1AA)=Sof(H1AB)=
 Sof(H1AC)=Sof(N1B)=Sof(C2B)=Sof(H2AA)=Sof(H2AB)=Sof(C3B)=Sof(H3AA)=Sof(H3AB)=
 Sof(C4B)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=1-FVAR(1)
 Sof(N1A)=Sof(C1A)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2A)=Sof(H2A)=Sof(H2B)=
 Sof(C3A)=Sof(H3A)=Sof(H3B)=Sof(C4A)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(H5AA)=
 Sof(H5AB)=Sof(H9AA)=Sof(H9AB)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C2A(H2A,H2B), C3A(H3A,H3B), C5(H5AA,H5AB), C5(H5BC,H5BD), C6(H6A,H6B), C7(H7A,
 H7B), C8(H8A,H8B), C9(H9AA,H9AB), C9(H9BC,H9BD), C2B(H2AA,H2AB), C3B(H3AA,H3AB)
5.b Idealised Me refined as rotating group:
 C1A(H1A,H1B,H1C), C4A(H4A,H4B,H4C), C1B(H1AA,H1AB,H1AC), C4B(H4AA,H4AB,H4AC)
;
_shelx_res_checksum              10998
_olex2_submission_special_instructions 'No special instructions were received'