#------------------------------------------------------------------------------
#$Date: 2016-02-21 11:56:54 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176809 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/04/2240437.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2240437
loop_
_publ_author_name
'Sun, Joobin'
'Heo, Jiyun'
'Yun, Hoseop'
_publ_section_title
;
 Crystal structure of the mixed-metal thiophosphate Nb~1.18~V~0.82~PS₁₀
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              278
_journal_page_last               280
_journal_paper_doi               10.1107/S2056989015003072
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'Nb1.18 V0.82 P S10'
_chemical_formula_sum            'Nb1.18 P S10 V0.82'
_chemical_formula_weight         502.97
_chemical_name_systematic
;
Niobium vanadium phosphorus decasulfide
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8472(4)
_cell_length_b                   13.6212(4)
_cell_length_c                   7.1972(3)
_cell_measurement_reflns_used    8753
_cell_measurement_temperature    290.0(10)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      3.17
_cell_volume                     1259.47(8)
_computing_cell_refinement
;
RAPID-AUTO (Rigaku, 2006)
;
_computing_data_collection
;
RAPID-AUTO (Rigaku, 2006)
;
_computing_data_reduction
;
RAPID-AUTO (Rigaku, 2006)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 1999)
;
_computing_publication_material
;
WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS2013 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      290.0(10)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID S'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0809
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            11897
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.994
_diffrn_reflns_theta_min         3.171
_exptl_absorpt_coefficient_mu    3.416
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5027
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Higashi, 1995)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.653
_exptl_crystal_description       needle
_exptl_crystal_F_000             969
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.043
_refine_diff_density_min         -1.064
_refine_ls_abs_structure_details
;
Flack (1983)
;
_refine_ls_abs_structure_Flack   0.64(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         2757
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0449
_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/[σ²(Fo²)+(0.0386P)²+1.1529P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.1034
_reflns_number_gt                2053
_reflns_number_total             2757
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            pj2018sup1.cf
_cod_data_source_block           I
_cod_database_code               2240437
_cod_database_fobs_code          2240437
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2.014
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
Nb Nb1 0.08230(7) 0.74603(8) 0.06349(16) 0.0193(3) Uani d 0.5889
V V1 0.08230(7) 0.74603(8) 0.06349(16) 0.0193(3) Uani d 0.4111
Nb Nb2 0.20780(7) 0.24841(8) 0.06671(16) 0.0183(3) Uani d 0.5856
V V2 0.20780(7) 0.24841(8) 0.06671(16) 0.0183(3) Uani d 0.4144
S S1 0.0601(2) 0.11893(17) 0.1005(4) 0.0233(6) Uani d 1
S S2 0.0647(2) 0.37577(18) 0.1107(4) 0.0258(6) Uani d 1
S S3 0.0727(2) 0.03201(19) 0.5538(4) 0.0285(6) Uani d 1
S S4 0.1930(2) 0.22558(19) 0.4241(4) 0.0284(6) Uani d 1
S S5 0.2221(2) 0.6344(2) 0.1672(4) 0.0277(7) Uani d 1
S S6 0.3292(2) 0.10963(19) 0.0949(4) 0.0284(7) Uani d 1
S S7 0.3483(2) 0.3569(2) 0.1743(4) 0.0292(7) Uani d 1
S S8 0.4267(2) 0.27029(19) 0.5806(4) 0.0284(6) Uani d 1
S S9 0.5644(2) 0.18846(18) 0.1448(4) 0.0275(6) Uani d 1
S S10 0.7986(2) 0.11500(19) 0.0879(5) 0.0275(7) Uani d 1
P P 0.0585(2) 0.15464(19) 0.3772(3) 0.0236(6) Uani d 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 '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_site_symmetry_1
_geom_angle
S8 P S4 3_456 117.17(16)
S8 P S1 3_456 106.08(17)
S4 P S1 . 105.61(17)
S8 P S3 3_456 112.75(17)
S4 P S3 . 101.85(16)
S1 P S3 . 113.40(15)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Nb1 S10 2_665 2.440(3)
Nb1 S7 4 2.450(3)
Nb1 S6 4 2.458(3)
Nb1 S5 . 2.469(3)
Nb1 S9 4 2.533(3)
Nb1 S2 2_565 2.537(3)
Nb1 S8 4_556 2.585(3)
Nb1 S1 2_565 2.608(3)
Nb1 Nb2 4 2.8549(13)
Nb2 S7 . 2.458(3)
Nb2 S6 . 2.459(3)
Nb2 S5 4_545 2.461(3)
Nb2 S10 3_455 2.462(3)
Nb2 S9 3_455 2.540(3)
Nb2 S2 . 2.547(3)
Nb2 S4 . 2.598(3)
Nb2 S1 . 2.602(3)
P S1 . 2.050(3)
P S3 . 2.107(3)
P S4 . 2.008(4)
P S8 3_456 2.002(4)
