Alkahest for V2VI3 Chalcogenides: Dissolution of Nine Bulk Semiconductors in a Diamine-Dithiol Solvent Mixture
David H. Webber; Richard L. Brutchey; Journal of the American Chemical Society 135 (2013) 15722–15725; doi:10.1021/ja4084336

data_4121002
_publ_contact_author_address
;
University of Southern California
Loker Hydrocarbon Research Institute and Department of Chemistry
Los Angeles, CA 90089
USA
;
_publ_contact_author_email       haiges@usc.edu
_publ_contact_author_name        'Ralf Haiges'
_publ_contact_author_phone       '+1 (213) 740-3197'
_publ_section_title
;
 Alkahest for V2VI3 Chalcogenides: Dissolution of Nine Bulk Semiconductors
 in a Diamine-Dithiol Solvent Mixture
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15722
_journal_page_last               15725
_journal_paper_doi               10.1021/ja4084336
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C2 H9 N2, 0.5(C2 H8 N2), 0.5(C2 H4 S2) '
_chemical_formula_sum            'C8 H30 N6 S2'
_chemical_formula_weight         274.50
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           'APEX2 v2013.4-1'
_cell_angle_alpha                90
_cell_angle_beta                 90.886(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.887(3)
_cell_length_b                   17.087(8)
_cell_length_c                   7.825(4)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      30.5456
_cell_measurement_theta_min      2.3883
_cell_volume                     787.0(7)
_computing_cell_refinement       'APEX2 v2013.4-1 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v2012.12.0.3'
_computing_data_reduction        'SAINT V8.30C (Bruker AXS, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXTL XT 2013/1 (Bruker AXS)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega- and phi-scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            18383
_diffrn_reflns_theta_full        30.56
_diffrn_reflns_theta_max         30.56
_diffrn_reflns_theta_min         2.38
_diffrn_source                   'fine-focus tube'
_exptl_absorpt_coefficient_mu    0.328
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS V2012/1'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_description       plate
_exptl_crystal_F_000             304
_exptl_crystal_size_max          0.533
_exptl_crystal_size_mid          0.315
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         2391
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0219
_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^)+(0.0296P)^2^+0.1721P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0611
_refine_ls_wR_factor_ref         0.0626
_reflns_number_gt                2241
_reflns_number_total             2391
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja4084336_si_002.cif
_cod_data_source_block           I
_cod_database_code               4121002