New Polymorph of Mo3S4 Prepared using a High-pressure Synthesis Technique: Crystal Structure, Electronic Property, and Band Calculation
Hiroshi Fukuoka; Kumi Masuoka; Teruhiko Hanaoka; Kei Inumaru; Inorganic Chemistry 52 (2013) 7918–7922; doi:10.1021/ic400423n

data_4335444
_publ_contact_author_address
'Hiroshima University, Higashi-Hiroshima 739-8527, Japan'
_publ_contact_author_name        'Hiroshi Fukuoka'
_publ_contact_author_phone       +81-82-424-7742
_publ_section_title
;
 New Polymorph of Mo3S4 Prepared using a High-pressure Synthesis
 Technique: Crystal Structure, Electronic Property, and Band Calculation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7918
_journal_page_last               7922
_journal_paper_doi               10.1021/ic400423n
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'Mo3 S4'
_chemical_formula_sum            'Mo3 S4'
_chemical_formula_weight         416.06
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.899(3)
_cell_angle_beta                 117.753(3)
_cell_angle_gamma                103.958(3)
_cell_formula_units_Z            2
_cell_length_a                   6.364(2)
_cell_length_b                   6.608(2)
_cell_length_c                   6.809(2)
_cell_measurement_reflns_used    800
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.81
_cell_measurement_theta_min      3.48
_cell_volume                     224.25(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 0.89
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker Apex-2'
_diffrn_measurement_method       'narrow-frame algorithm'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0069
_diffrn_reflns_av_sigmaI/netI    0.0105
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            933
_diffrn_reflns_theta_full        23.47
_diffrn_reflns_theta_max         23.47
_diffrn_reflns_theta_min         3.48
_exptl_absorpt_coefficient_mu    9.923
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    6.161
_exptl_crystal_description       'a rectangular parallelepiped'
_exptl_crystal_F_000             380
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.731
_refine_diff_density_min         -1.525
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     64
_refine_ls_number_reflns         652
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0218
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+2.1932P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0585
_refine_ls_wR_factor_ref         0.0589
_reflns_number_gt                629
_reflns_number_total             652
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400423n_si_001.cif
_cod_data_source_block           Mo3S4
_cod_original_cell_volume        224.28(13)
_cod_database_code               4335444