#------------------------------------------------------------------------------
#$Date: 2016-01-15 10:04:49 +0200 (Fri, 15 Jan 2016) $
#$Revision: 174504 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/38/7223891.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_7223891
loop_
_publ_author_name
'Sui, Lifang'
'Zhang, Xian'
'Tian, Zhangliu'
'Huang, Rongtie'
'Zhang, Hui'
'Cheng, Jinrong'
'Huang, Fu Qiang'
_publ_section_title
;
 Synthesis, Crystal Structure and Physical Properties of FeV4S8 and
 KFe2V8S16
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA22619H
_journal_year                    2016
_chemical_formula_moiety         '2(Fe S8 V4), 2(K0.50) '
_chemical_formula_sum            'Fe2 K S16 V8'
_chemical_formula_weight         1071.28
_chemical_name_common            'Potassium iron Vanadium Sulfur'
_chemical_name_systematic
;
Potassium iron Vanadium Sulfur
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-06-17 deposited with the CCDC.
2016-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.824(12)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   17.465(5)
_cell_length_b                   3.2929(11)
_cell_length_c                   8.473(3)
_cell_measurement_reflns_used    5646
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.463
_cell_measurement_theta_min      2.402
_cell_volume                     473.2(3)
_computing_cell_refinement       'SHELXL-2014 (Sheldrick, 2014)'
_computing_data_collection       'SHELXL-2014 (Sheldrick, 2014)'
_computing_data_reduction        'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8Quest'
_diffrn_measurement_method       'ω and φ'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_unetI/netI     0.0117
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7878
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.475
_diffrn_reflns_theta_min         2.402
_exptl_absorpt_coefficient_mu    7.215
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.759
_exptl_crystal_description       polyhedra
_exptl_crystal_F_000             511
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.058
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.57
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       0.0030(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         638
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0171
_refine_ls_R_factor_gt           0.0161
_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)+(0.0209P)²+1.1975P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0423
_refine_ls_wR_factor_ref         0.0427
_reflns_Friedel_coverage         0.000
_reflns_number_gt                612
_reflns_number_total             638
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ra22619h2.cif
_cod_data_source_block           C2-m
_cod_original_formula_sum        ' Fe2 K S16 V8'
_cod_database_code               7223891
_audit_block_doi                 10.5517/cc1j7d49
_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.
;
_shelx_estimated_absorpt_t_min   0.680
_shelx_estimated_absorpt_t_max   0.931
_shelxl_version_number           2014-3
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'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
K K 0.0000 0.0000 0.0000 0.0235(4) Uani 0.5 4 d S T P
V1 V 0.28978(2) 0.5000 0.14231(5) 0.01556(14) Uani 0.5 2 d S T P
Fe1 Fe 0.28978(2) 0.5000 0.14231(5) 0.01556(14) Uani 0.5 2 d S T P
V2 V 0.0000 0.5000 0.5000 0.01343(16) Uani 1 4 d S T P
V3 V 0.14927(3) 0.0000 0.48986(5) 0.01126(13) Uani 1 2 d S T P
S1 S 0.16100(4) 0.5000 0.00184(7) 0.01202(16) Uani 1 2 d S T P
S2 S 0.08517(4) 0.5000 0.31567(7) 0.01166(15) Uani 1 2 d S T P
S3 S 0.42648(3) 0.5000 0.32375(7) 0.01060(15) Uani 1 2 d S T P
S4 S 0.23997(3) -0.5000 0.65716(7) 0.01006(15) Uani 1 2 d S T P
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'
K K 0.2009 0.2494 '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'
Fe Fe 0.3463 0.8444 '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
S2 K S2 180.0 . 5
S2 K S2 117.85(3) . 5_565
S2 K S2 62.15(3) 5 5_565
S2 K S2 62.15(3) . 1_545
S2 K S2 117.85(3) 5 1_545
S2 K S2 180.00(2) 5_565 1_545
S2 K S1 119.62(2) . 5
S2 K S1 60.38(2) 5 5
S2 K S1 91.60(2) 5_565 5
S2 K S1 88.40(2) 1_545 5
S2 K S1 88.40(2) . 5_565
S2 K S1 91.60(2) 5 5_565
S2 K S1 60.38(2) 5_565 5_565
S2 K S1 119.62(2) 1_545 5_565
S1 K S1 60.77(2) 5 5_565
S2 K S1 91.60(2) . 1_545
S2 K S1 88.40(2) 5 1_545
S2 K S1 119.62(2) 5_565 1_545
S2 K S1 60.38(2) 1_545 1_545
S1 K S1 119.23(2) 5 1_545
S1 K S1 180.000(11) 5_565 1_545
S2 K S1 60.38(2) . .
S2 K S1 119.62(2) 5 .
S2 K S1 88.40(2) 5_565 .
S2 K S1 91.60(2) 1_545 .
S1 K S1 180.0 5 .
S1 K S1 119.23(3) 5_565 .
S1 K S1 60.77(3) 1_545 .
S2 K S3 120.11(2) . 7
S2 K S3 59.89(2) 5 7
S2 K S3 59.89(2) 5_565 7
S2 K S3 120.11(2) 1_545 7
S1 K S3 120.268(18) 5 7
S1 K S3 120.268(17) 5_565 7
S1 K S3 59.732(18) 1_545 7
S1 K S3 59.732(18) . 7
S2 K S3 59.89(2) . 3_445
S2 K S3 120.11(2) 5 3_445
S2 K S3 120.11(2) 5_565 3_445
S2 K S3 59.89(2) 1_545 3_445
S1 K S3 59.732(18) 5 3_445
S1 K S3 59.732(18) 5_565 3_445
S1 K S3 120.268(17) 1_545 3_445
S1 K S3 120.268(18) . 3_445
K K S3 90.0 1_545 3_445
K K S3 90.0 1_565 3_445
S3 K S3 180.00(2) 7 3_445
S1 V1 S1 99.65(3) . 7
S1 V1 S1 99.65(3) . 7_565
S1 V1 S1 89.78(3) 7 7_565
S1 V1 S4 90.89(3) . 7_556
S1 V1 S4 168.48(3) 7 7_556
S1 V1 S4 93.05(3) 7_565 7_556
S1 V1 S4 90.89(3) . 7_546
S1 V1 S4 93.05(3) 7 7_546
S1 V1 S4 168.48(3) 7_565 7_546
S4 V1 S4 82.07(3) 7_556 7_546
S1 V1 S3 174.00(3) . .
S1 V1 S3 84.56(3) 7 .
S1 V1 S3 84.56(3) 7_565 .
S4 V1 S3 84.60(3) 7_556 .
S4 V1 S3 84.60(3) 7_546 .
S3 V2 S3 180.0 7_566 3_445
S3 V2 S3 87.46(3) 7_566 7_556
S3 V2 S3 92.54(3) 3_445 7_556
S3 V2 S3 92.54(3) 7_566 3_455
S3 V2 S3 87.46(3) 3_445 3_455
S3 V2 S3 180.0 7_556 3_455
S3 V2 S2 85.25(3) 7_566 5_566
S3 V2 S2 94.75(3) 3_445 5_566
S3 V2 S2 85.25(3) 7_556 5_566
S3 V2 S2 94.75(3) 3_455 5_566
S3 V2 S2 94.75(3) 7_566 .
S3 V2 S2 85.25(3) 3_445 .
S3 V2 S2 94.75(3) 7_556 .
S3 V2 S2 85.25(3) 3_455 .
S2 V2 S2 180.0 5_566 .
S3 V3 S2 99.71(3) 7_556 1_545
S3 V3 S2 99.71(3) 7_556 .
S2 V3 S2 90.74(4) 1_545 .
S3 V3 S4 90.07(3) 7_556 1_565
S2 V3 S4 169.19(3) 1_545 1_565
S2 V3 S4 92.16(3) . 1_565
S3 V3 S4 90.07(3) 7_556 .
S2 V3 S4 92.17(3) 1_545 .
S2 V3 S4 169.18(3) . .
S4 V3 S4 83.15(3) 1_565 .
S3 V3 S4 166.41(3) 7_556 7_546
S2 V3 S4 89.79(3) 1_545 7_546
S2 V3 S4 89.79(3) . 7_546
S4 V3 S4 79.81(3) 1_565 7_546
S4 V3 S4 79.81(3) . 7_546
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K S2 3.1899(9) .
K S2 3.1899(9) 5
K S2 3.1899(9) 5_565
K S2 3.1899(9) 1_545
K S1 3.2553(9) 5
K S1 3.2553(9) 5_565
K S1 3.2553(9) 1_545
K S1 3.2553(9) .
K K 3.2929(11) 1_545
K K 3.2929(11) 1_565
K S3 3.2949(11) 7
K S3 3.2949(11) 3_445
V1 S1 2.2794(10) .
V1 S1 2.3330(7) 7
V1 S1 2.3330(7) 7_565
V1 S4 2.5078(8) 7_556
V1 S4 2.5078(8) 7_546
V1 S3 2.5117(10) .
V1 Fe1 2.9759(10) 7
V1 V1 2.9759(10) 7
V1 V1 2.9759(10) 7_565
V1 V3 3.0431(12) 7_556
V2 S3 2.3819(7) 7_566
V2 S3 2.3819(7) 3_445
V2 S3 2.3819(7) 7_556
V2 S3 2.3819(7) 3_455
V2 S2 2.4003(8) 5_566
V2 S2 2.4004(8) .
V2 V3 3.1019(8) .
V2 V3 3.1020(8) 1_565
V2 V3 3.1020(8) 5_556
V2 V3 3.1020(8) 5_566
V3 S3 2.2897(9) 7_556
V3 S2 2.3136(7) 1_545
V3 S2 2.3136(7) .
V3 S4 2.4811(7) 1_565
V3 S4 2.4812(7) .
V3 S4 2.5387(9) 7_546
V3 V1 3.0431(12) 7_556
V3 V2 3.1019(8) 1_545
S1 V1 2.3330(7) 7
S1 V1 2.3330(7) 7_565
S1 K 3.2553(9) 1_565
S2 V3 2.3136(7) 1_565
S2 K 3.1899(9) 1_565
S3 V3 2.2897(9) 7_556
S3 V2 2.3819(7) 3
S3 V2 2.3819(7) 3_545
S3 K 3.2949(11) 3
S4 V3 2.4811(7) 1_545
S4 V1 2.5078(8) 7_556
S4 V1 2.5078(8) 7_546
S4 V3 2.5386(9) 7_546
