#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:49:05 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179457 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/54/4335444.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4335444
loop_
_publ_author_name
'Hiroshi Fukuoka'
'Kumi Masuoka'
'Teruhiko Hanaoka'
'Kei Inumaru'
_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/[σ²(Fo²)+(0.0282P)²+2.1932P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
Mo1 Mo 0.27920(10) 0.00147(8) 0.50321(9) 0.0083(2) Uani 1 1 d
Mo2 Mo 0.45364(10) 0.48276(8) 1.18129(9) 0.0048(2) Uani 1 1 d
Mo3 Mo -0.02510(10) 0.48563(8) 1.19147(9) 0.0049(2) Uani 1 1 d
S1 S 0.5307(3) 0.2127(2) 0.9482(3) 0.0056(3) Uani 1 1 d
S2 S 0.0542(3) 0.2693(3) 0.4722(3) 0.0057(3) Uani 1 1 d
S3 S -0.0163(3) -0.2054(2) 0.0635(3) 0.0059(3) Uani 1 1 d
S4 S 0.4454(3) -0.2851(3) 0.5320(3) 0.0053(3) Uani 1 1 d
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
S4 Mo1 S4 107.00(5) 2_656 .
S4 Mo1 S3 92.07(5) 2_656 .
S4 Mo1 S3 91.47(5) . .
S4 Mo1 S1 91.92(5) 2_656 .
S4 Mo1 S1 93.00(5) . .
S3 Mo1 S1 172.88(5) . .
S4 Mo1 S2 80.72(6) 2_656 .
S4 Mo1 S2 172.26(5) . .
S3 Mo1 S2 87.59(5) . .
S1 Mo1 S2 87.25(5) . .
S4 Mo1 S2 171.85(5) 2_656 2_556
S4 Mo1 S2 81.07(6) . 2_556
S3 Mo1 S2 86.45(5) . 2_556
S1 Mo1 S2 88.77(5) . 2_556
S2 Mo1 S2 91.20(6) . 2_556
S4 Mo1 Mo1 53.60(4) 2_656 2_656
S4 Mo1 Mo1 53.40(4) . 2_656
S3 Mo1 Mo1 92.97(5) . 2_656
S1 Mo1 Mo1 94.14(4) . 2_656
S2 Mo1 Mo1 134.32(4) . 2_656
S2 Mo1 Mo1 134.45(5) 2_556 2_656
S4 Mo1 Mo3 129.95(4) 2_656 1_544
S4 Mo1 Mo3 53.07(4) . 1_544
S3 Mo1 Mo3 50.27(4) . 1_544
S1 Mo1 Mo3 129.65(4) . 1_544
S2 Mo1 Mo3 121.55(5) . 1_544
S2 Mo1 Mo3 53.97(4) 2_556 1_544
Mo1 Mo1 Mo3 91.91(3) 2_656 1_544
S4 Mo1 Mo2 53.82(4) 2_656 2_667
S4 Mo1 Mo2 130.20(5) . 2_667
S3 Mo1 Mo2 129.77(4) . 2_667
S1 Mo1 Mo2 49.57(4) . 2_667
S2 Mo1 Mo2 54.80(4) . 2_667
S2 Mo1 Mo2 121.89(4) 2_556 2_667
Mo1 Mo1 Mo2 92.74(3) 2_656 2_667
Mo3 Mo1 Mo2 175.34(2) 1_544 2_667
S3 Mo2 S1 108.01(6) 2_556 2_667
S3 Mo2 S1 85.16(6) 2_556 .
S1 Mo2 S1 107.07(5) 2_667 .
S3 Mo2 S4 88.82(5) 2_556 2_657
S1 Mo2 S4 158.76(6) 2_667 2_657
S1 Mo2 S4 86.71(6) . 2_657
S3 Mo2 S4 98.76(5) 2_556 1_566
S1 Mo2 S4 89.98(6) 2_667 1_566
S1 Mo2 S4 160.50(5) . 1_566
S4 Mo2 S4 74.34(6) 2_657 1_566
S3 Mo2 S2 164.49(5) 2_556 2_667
S1 Mo2 S2 86.76(5) 2_667 2_667
S1 Mo2 S2 95.18(6) . 2_667
S4 Mo2 S2 75.74(5) 2_657 2_667
S4 Mo2 S2 75.98(5) 1_566 2_667
S3 Mo2 Mo3 54.16(4) 2_556 2_567
S1 Mo2 Mo3 53.86(4) 2_667 2_567
S1 Mo2 Mo3 101.29(5) . 2_567
S4 Mo2 Mo3 140.60(4) 2_657 2_567
S4 Mo2 Mo3 96.39(5) 1_566 2_567
S2 Mo2 Mo3 140.21(4) 2_667 2_567
S3 Mo2 Mo2 100.86(5) 2_556 2_667
S1 Mo2 Mo2 53.72(4) 2_667 2_667
S1 Mo2 Mo2 53.35(4) . 2_667
S4 Mo2 Mo2 137.21(5) 2_657 2_667
S4 Mo2 Mo2 142.62(5) 1_566 2_667
S2 Mo2 Mo2 91.64(5) 2_667 2_667
Mo3 Mo2 Mo2 70.74(3) 2_567 2_667
S3 Mo2 Mo1 134.52(4) 2_556 2_667
S1 Mo2 Mo1 51.90(4) 2_667 2_667
S1 Mo2 Mo1 136.69(4) . 2_667
S4 Mo2 Mo1 107.03(5) 2_657 2_667
S4 Mo2 Mo1 49.14(4) 1_566 2_667
S2 Mo2 Mo1 51.88(3) 2_667 2_667
Mo3 Mo2 Mo1 93.39(3) 2_567 2_667
Mo2 Mo2 Mo1 95.50(3) 2_667 2_667
S3 Mo2 Mo3 49.46(4) 2_556 .
S1 Mo2 Mo3 91.03(4) 2_667 .
S1 Mo2 Mo3 134.59(4) . .
S4 Mo2 Mo3 90.36(4) 2_657 .
S4 Mo2 Mo3 51.89(4) 1_566 .
S2 Mo2 Mo3 127.84(4) 2_667 .
Mo3 Mo2 Mo3 56.64(3) 2_567 .
Mo2 Mo2 Mo3 127.37(3) 2_667 .
Mo1 Mo2 Mo3 87.23(2) 2_667 .
S3 Mo3 S1 82.40(6) 2_556 1_455
S3 Mo3 S3 107.79(5) 2_556 1_566
S1 Mo3 S3 106.66(6) 1_455 1_566
S3 Mo3 S4 99.69(6) 2_556 1_566
S1 Mo3 S4 162.61(5) 1_455 1_566
S3 Mo3 S4 89.24(5) 1_566 1_566
S3 Mo3 S2 166.20(5) 2_556 2_567
S1 Mo3 S2 96.11(5) 1_455 2_567
S3 Mo3 S2 85.82(5) 1_566 2_567
S4 Mo3 S2 77.71(5) 1_566 2_567
S3 Mo3 S2 88.08(6) 2_556 1_556
S1 Mo3 S2 86.35(5) 1_455 1_556
S3 Mo3 S2 160.41(5) 1_566 1_556
S4 Mo3 S2 76.51(5) 1_566 1_556
S2 Mo3 S2 78.13(6) 2_567 1_556
S3 Mo3 Mo3 54.40(4) 2_556 2_567
S1 Mo3 Mo3 97.66(5) 1_455 2_567
S3 Mo3 Mo3 53.39(4) 1_566 2_567
S4 Mo3 Mo3 97.50(5) 1_566 2_567
S2 Mo3 Mo3 139.15(5) 2_567 2_567
S2 Mo3 Mo3 140.92(5) 1_556 2_567
S3 Mo3 Mo2 97.41(5) 2_556 2_567
S1 Mo3 Mo2 53.48(4) 1_455 2_567
S3 Mo3 Mo2 53.20(4) 1_566 2_567
S4 Mo3 Mo2 142.05(4) 1_566 2_567
S2 Mo3 Mo2 92.60(4) 2_567 2_567
S2 Mo3 Mo2 137.85(4) 1_556 2_567
Mo3 Mo3 Mo2 66.25(3) 2_567 2_567
S3 Mo3 Mo1 135.31(4) 2_556 1_566
S1 Mo3 Mo1 137.49(4) 1_455 1_566
S3 Mo3 Mo1 51.12(4) 1_566 1_566
S4 Mo3 Mo1 49.49(4) 1_566 1_566
S2 Mo3 Mo1 52.29(4) 2_567 1_566
S2 Mo3 Mo1 109.46(5) 1_556 1_566
Mo3 Mo3 Mo1 93.63(3) 2_567 1_566
Mo2 Mo3 Mo1 95.67(3) 2_567 1_566
S3 Mo3 Mo2 49.50(4) 2_556 .
S1 Mo3 Mo2 131.89(4) 1_455 .
S3 Mo3 Mo2 90.30(4) 1_566 .
S4 Mo3 Mo2 52.82(4) 1_566 .
S2 Mo3 Mo2 130.44(4) 2_567 .
S2 Mo3 Mo2 91.61(4) 1_556 .
Mo3 Mo3 Mo2 57.11(2) 2_567 .
Mo2 Mo3 Mo2 123.36(3) 2_567 .
Mo1 Mo3 Mo2 88.12(2) 1_566 .
Mo2 S1 Mo2 72.93(5) 2_667 .
Mo2 S1 Mo3 72.66(5) 2_667 1_655
Mo2 S1 Mo3 86.52(6) . 1_655
Mo2 S1 Mo1 78.53(5) 2_667 .
Mo2 S1 Mo1 128.48(6) . .
Mo3 S1 Mo1 124.29(6) 1_655 .
Mo1 S2 Mo1 88.80(6) . 2_556
Mo1 S2 Mo3 126.91(6) . 2_567
Mo1 S2 Mo3 73.74(5) 2_556 2_567
Mo1 S2 Mo3 126.98(6) . 1_554
Mo1 S2 Mo3 127.91(6) 2_556 1_554
Mo3 S2 Mo3 101.87(6) 2_567 1_554
Mo1 S2 Mo2 73.32(5) . 2_667
Mo1 S2 Mo2 126.81(6) 2_556 2_667
Mo3 S2 Mo2 78.29(5) 2_567 2_667
Mo3 S2 Mo2 101.43(6) 1_554 2_667
Mo3 S3 Mo2 81.05(5) 2_556 2_556
Mo3 S3 Mo3 72.21(5) 2_556 1_544
Mo2 S3 Mo3 72.64(5) 2_556 1_544
Mo3 S3 Mo1 126.41(7) 2_556 .
Mo2 S3 Mo1 130.82(6) 2_556 .
Mo3 S3 Mo1 78.61(5) 1_544 .
Mo1 S4 Mo1 73.00(5) 2_656 .
Mo1 S4 Mo3 120.40(6) 2_656 1_544
Mo1 S4 Mo3 77.44(5) . 1_544
Mo1 S4 Mo2 131.71(7) 2_656 2_657
Mo1 S4 Mo2 132.71(6) . 2_657
Mo3 S4 Mo2 106.32(6) 1_544 2_657
Mo1 S4 Mo2 77.04(5) 2_656 1_544
Mo1 S4 Mo2 120.36(6) . 1_544
Mo3 S4 Mo2 75.29(5) 1_544 1_544
Mo2 S4 Mo2 105.66(6) 2_657 1_544
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 S4 2.3805(16) 2_656
Mo1 S4 2.3867(17) .
Mo1 S3 2.4329(17) .
Mo1 S1 2.4629(17) .
Mo1 S2 2.5191(16) .
Mo1 S2 2.5249(16) 2_556
Mo1 Mo1 2.8358(14) 2_656
Mo1 Mo3 3.0639(11) 1_544
Mo1 Mo2 3.0672(11) 2_667
Mo2 S3 2.3741(17) 2_556
Mo2 S1 2.3822(16) 2_667
Mo2 S1 2.3938(16) .
Mo2 S4 2.5279(16) 2_657
Mo2 S4 2.5405(16) 1_566
Mo2 S2 2.6165(17) 2_667
Mo2 Mo3 2.8297(10) 2_567
Mo2 Mo2 2.8386(12) 2_667
Mo2 Mo1 3.0672(11) 2_667
Mo2 Mo3 3.0843(12) .
Mo3 S3 2.3726(16) 2_556
Mo3 S1 2.3941(17) 1_455
Mo3 S3 2.4035(16) 1_566
Mo3 S4 2.5091(17) 1_566
Mo3 S2 2.5808(16) 2_567
Mo3 S2 2.5916(16) 1_556
Mo3 Mo3 2.8146(13) 2_567
Mo3 Mo2 2.8297(10) 2_567
Mo3 Mo1 3.0639(11) 1_566
S1 Mo2 2.3823(16) 2_667
S1 Mo3 2.3941(17) 1_655
S2 Mo1 2.5249(16) 2_556
S2 Mo3 2.5808(16) 2_567
S2 Mo3 2.5916(16) 1_554
S2 Mo2 2.6165(17) 2_667
S3 Mo3 2.3726(16) 2_556
S3 Mo2 2.3740(17) 2_556
S3 Mo3 2.4035(16) 1_544
S4 Mo1 2.3805(16) 2_656
S4 Mo3 2.5091(16) 1_544
S4 Mo2 2.5279(16) 2_657
S4 Mo2 2.5405(16) 1_544
