#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:46:46 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179077 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/39/4303995.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_4303995
loop_
_publ_author_name
'Danielle L. Gray'
'Gary J. Long'
'Fernande Grandjean'
'Raphaël P. Hermann'
'James A. Ibers'
_publ_section_title
;
Syntheses, Structure, and a Mössbauer and Magnetic Study of Ba4Fe2I5S4
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              94
_journal_page_last               100
_journal_paper_doi               10.1021/ic701085c
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'Ba4 Fe2 I5 S4'
_chemical_formula_weight         1423.80
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.7583(13)
_cell_length_b                   13.7583(13)
_cell_length_c                   5.1261(7)
_cell_measurement_reflns_used    4575
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.266
_cell_measurement_theta_min      3.309
_cell_volume                     970.32(19)
_computing_cell_refinement       'SMART Version 5.054 (Bruker, 2000)'
_computing_data_collection       'SMART Version 5.054 (Bruker, 2000)'
_computing_data_reduction        'Saint-Plus Version 6.45 (Bruker, 2003)'
_computing_molecular_graphics    'Crystalmaker for Windows version 1.3 (2005)'
_computing_publication_material  'SHELXTL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'Bruker Smart 1000 CCD'
_diffrn_measurement_method       ω
_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  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0133
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            5782
_diffrn_reflns_theta_full        28.71
_diffrn_reflns_theta_max         28.71
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        <2
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.800
_exptl_absorpt_correction_T_max  0.60575
_exptl_absorpt_correction_T_min  0.20095
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'faces indexed'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.873
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       needle
_exptl_crystal_F_000             1210
_exptl_crystal_size_max          0.314
_exptl_crystal_size_mid          0.032
_exptl_crystal_size_min          0.030
_refine_diff_density_max         3.503
_refine_diff_density_min         -1.427
_refine_diff_density_rms         0.360
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.302
_refine_ls_matrix_type           full
_refine_ls_number_parameters     23
_refine_ls_number_reflns         650
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.302
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc 
 [1.00000+0.00000exp(0.00(sinθ/λ)²)]/ 
   [σ²(Fo²)+0.0000+0.0000*P+(0.0300P)²+0.0000sinθ/λ] 
 where P = 1.00000Fo² + 0.00000Fc² 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.0904
_reflns_number_gt                632
_reflns_number_total             650
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701085c.cif
_cod_data_source_block           Ba4Fe2S4I5
_cod_database_code               4303995
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
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
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ba1 Ba 0.24801(4) 0.06079(4) 0.0000 0.0125(2) Uani 1 2 d S . .
Fe1 Fe 0.0000 0.5000 0.2500 0.0095(4) Uani 1 4 d S . .
I1 I 0.0000 0.0000 0.0000 0.0183(3) Uani 1 8 d S . .
I2 I 0.36929(4) 0.29706(4) 0.0000 0.0143(2) Uani 1 2 d S . .
S1 S 0.10360(15) 0.41200(15) 0.0000 0.0107(4) Uani 1 2 d S . .
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ba Ba -0.3244 2.2819 '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
_geom_angle_publ_flag
S1 Ba1 S1 69.09(6) 11 13 ?
S1 Ba1 S1 69.09(6) 11 13_554 ?
S1 Ba1 S1 102.00(6) 13 13_554 ?
S1 Ba1 I1 121.16(4) 11 . ?
S1 Ba1 I1 128.92(3) 13 . ?
S1 Ba1 I1 128.92(3) 13_554 . ?
S1 Ba1 I2 134.442(10) 11 13 ?
S1 Ba1 I2 70.31(3) 13 13 ?
S1 Ba1 I2 140.17(4) 13_554 13 ?
I1 Ba1 I2 72.204(12) . 13 ?
S1 Ba1 I2 134.442(10) 11 13_554 ?
S1 Ba1 I2 140.17(4) 13 13_554 ?
S1 Ba1 I2 70.31(3) 13_554 13_554 ?
I1 Ba1 I2 72.204(12) . 13_554 ?
I2 Ba1 I2 90.61(2) 13 13_554 ?
S1 Ba1 I2 107.90(4) 11 . ?
S1 Ba1 I2 67.44(4) 13 . ?
S1 Ba1 I2 67.44(4) 13_554 . ?
I1 Ba1 I2 130.943(18) . . ?
I2 Ba1 I2 73.847(15) 13 . ?
I2 Ba1 I2 73.847(15) 13_554 . ?
S1 Ba1 I2 67.49(3) 11 7_544 ?
S1 Ba1 I2 135.85(4) 13 7_544 ?
S1 Ba1 I2 69.44(3) 13_554 7_544 ?
I1 Ba1 I2 70.743(12) . 7_544 ?
I2 Ba1 I2 142.92(2) 13 7_544 ?
I2 Ba1 I2 79.640(16) 13_554 7_544 ?
I2 Ba1 I2 134.810(11) . 7_544 ?
S1 Ba1 I2 67.49(3) 11 7_545 ?
S1 Ba1 I2 69.44(3) 13 7_545 ?
S1 Ba1 I2 135.85(4) 13_554 7_545 ?
I1 Ba1 I2 70.743(12) . 7_545 ?
I2 Ba1 I2 79.640(16) 13 7_545 ?
I2 Ba1 I2 142.92(2) 13_554 7_545 ?
I2 Ba1 I2 134.810(11) . 7_545 ?
I2 Ba1 I2 86.879(18) 7_544 7_545 ?
S1 Ba1 Fe1 36.64(3) 11 13 ?
S1 Ba1 Fe1 36.48(3) 13 13 ?
S1 Ba1 Fe1 73.83(3) 13_554 13 ?
I1 Ba1 Fe1 146.722(13) . 13 ?
I2 Ba1 Fe1 106.788(12) 13 13 ?
I2 Ba1 Fe1 140.319(15) 13_554 13 ?
I2 Ba1 Fe1 77.206(12) . 13 ?
I2 Ba1 Fe1 103.222(15) 7_544 13 ?
I2 Ba1 Fe1 76.331(12) 7_545 13 ?
S1 Ba1 Fe1 36.64(3) 11 5_544 ?
S1 Ba1 Fe1 73.83(3) 13 5_544 ?
S1 Ba1 Fe1 36.48(3) 13_554 5_544 ?
I1 Ba1 Fe1 146.722(13) . 5_544 ?
I2 Ba1 Fe1 140.319(15) 13 5_544 ?
I2 Ba1 Fe1 106.788(12) 13_554 5_544 ?
I2 Ba1 Fe1 77.206(12) . 5_544 ?
I2 Ba1 Fe1 76.331(12) 7_544 5_544 ?
I2 Ba1 Fe1 103.222(15) 7_545 5_544 ?
Fe1 Ba1 Fe1 39.530(8) 13 5_544 ?
S1 Fe1 S1 108.64(3) 7 9_565 ?
S1 Fe1 S1 111.16(6) 7 15_455 ?
S1 Fe1 S1 108.64(3) 9_565 15_455 ?
S1 Fe1 S1 108.63(3) 7 . ?
S1 Fe1 S1 111.16(6) 9_565 . ?
S1 Fe1 S1 108.63(3) 15_455 . ?
S1 Fe1 Fe1 55.58(3) 7 9_566 ?
S1 Fe1 Fe1 124.42(3) 9_565 9_566 ?
S1 Fe1 Fe1 55.58(3) 15_455 9_566 ?
S1 Fe1 Fe1 124.42(3) . 9_566 ?
S1 Fe1 Fe1 124.42(3) 7 9_565 ?
S1 Fe1 Fe1 55.58(3) 9_565 9_565 ?
S1 Fe1 Fe1 124.42(3) 15_455 9_565 ?
S1 Fe1 Fe1 55.58(3) . 9_565 ?
Fe1 Fe1 Fe1 180.0 9_566 9_565 ?
S1 Fe1 Ba1 152.15(5) 7 3 ?
S1 Fe1 Ba1 99.13(5) 9_565 3 ?
S1 Fe1 Ba1 59.88(4) 15_455 3 ?
S1 Fe1 Ba1 57.25(5) . 3 ?
Fe1 Fe1 Ba1 109.765(4) 9_566 3 ?
Fe1 Fe1 Ba1 70.235(4) 9_565 3 ?
S1 Fe1 Ba1 57.25(5) 7 13 ?
S1 Fe1 Ba1 152.15(5) 9_565 13 ?
S1 Fe1 Ba1 99.13(5) 15_455 13 ?
S1 Fe1 Ba1 59.87(4) . 13 ?
Fe1 Fe1 Ba1 70.235(4) 9_566 13 ?
Fe1 Fe1 Ba1 109.765(4) 9_565 13 ?
Ba1 Fe1 Ba1 96.566(3) 3 13 ?
S1 Fe1 Ba1 59.88(4) 7 11_565 ?
S1 Fe1 Ba1 57.25(5) 9_565 11_565 ?
S1 Fe1 Ba1 152.15(5) 15_455 11_565 ?
S1 Fe1 Ba1 99.13(5) . 11_565 ?
Fe1 Fe1 Ba1 109.765(4) 9_566 11_565 ?
Fe1 Fe1 Ba1 70.235(4) 9_565 11_565 ?
Ba1 Fe1 Ba1 140.470(8) 3 11_565 ?
Ba1 Fe1 Ba1 96.566(3) 13 11_565 ?
S1 Fe1 Ba1 99.13(5) 7 5_455 ?
S1 Fe1 Ba1 59.88(4) 9_565 5_455 ?
S1 Fe1 Ba1 57.25(5) 15_455 5_455 ?
S1 Fe1 Ba1 152.15(5) . 5_455 ?
Fe1 Fe1 Ba1 70.235(4) 9_566 5_455 ?
Fe1 Fe1 Ba1 109.765(4) 9_565 5_455 ?
Ba1 Fe1 Ba1 96.566(3) 3 5_455 ?
Ba1 Fe1 Ba1 140.470(8) 13 5_455 ?
Ba1 Fe1 Ba1 96.566(3) 11_565 5_455 ?
Ba1 I1 Ba1 90.0 9 11 ?
Ba1 I1 Ba1 90.0 9 3 ?
Ba1 I1 Ba1 180.000(16) 11 3 ?
Ba1 I1 Ba1 180.0 9 . ?
Ba1 I1 Ba1 90.0 11 . ?
Ba1 I1 Ba1 90.0 3 . ?
Ba1 I2 Ba1 90.62(2) 13 13_554 ?
Ba1 I2 Ba1 106.153(15) 13 . ?
Ba1 I2 Ba1 106.153(15) 13_554 . ?
Ba1 I2 Ba1 85.285(14) 13 15 ?
Ba1 I2 Ba1 153.56(2) 13_554 15 ?
Ba1 I2 Ba1 100.066(17) . 15 ?
Ba1 I2 Ba1 153.56(2) 13 15_554 ?
Ba1 I2 Ba1 85.285(14) 13_554 15_554 ?
Ba1 I2 Ba1 100.066(17) . 15_554 ?
Ba1 I2 Ba1 86.878(19) 15 15_554 ?
Fe1 S1 Fe1 68.84(6) 9_565 . ?
Fe1 S1 Ba1 86.10(6) 9_565 3 ?
Fe1 S1 Ba1 86.10(6) . 3 ?
Fe1 S1 Ba1 140.16(8) 9_565 13 ?
Fe1 S1 Ba1 83.64(3) . 13 ?
Ba1 S1 Ba1 121.22(4) 3 13 ?
Fe1 S1 Ba1 83.64(3) 9_565 13_554 ?
Fe1 S1 Ba1 140.16(8) . 13_554 ?
Ba1 S1 Ba1 121.22(4) 3 13_554 ?
Ba1 S1 Ba1 102.00(6) 13 13_554 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ba1 S1 3.195(2) 11 ?
Ba1 S1 3.2981(14) 13 ?
Ba1 S1 3.2981(14) 13_554 ?
Ba1 I1 3.5132(6) . ?
Ba1 I2 3.6054(6) 13 ?
Ba1 I2 3.6054(6) 13_554 ?
Ba1 I2 3.6539(8) . ?
Ba1 I2 3.7276(6) 7_544 ?
Ba1 I2 3.7276(6) 7_545 ?
Ba1 Fe1 3.7896(6) 13 ?
Ba1 Fe1 3.7896(6) 5_544 ?
Fe1 S1 2.2671(17) 7 ?
Fe1 S1 2.2671(17) 9_565 ?
Fe1 S1 2.2671(17) 15_455 ?
Fe1 S1 2.2671(17) . ?
Fe1 Fe1 2.5630(4) 9_566 ?
Fe1 Fe1 2.5631(4) 9_565 ?
Fe1 Ba1 3.7897(6) 3 ?
Fe1 Ba1 3.7897(6) 13 ?
Fe1 Ba1 3.7897(6) 11_565 ?
Fe1 Ba1 3.7897(6) 5_455 ?
I1 Ba1 3.5132(6) 9 ?
I1 Ba1 3.5132(6) 11 ?
I1 Ba1 3.5132(6) 3 ?
I2 Ba1 3.6054(6) 13 ?
I2 Ba1 3.6054(6) 13_554 ?
I2 Ba1 3.7276(6) 15 ?
I2 Ba1 3.7276(6) 15_554 ?
S1 Fe1 2.2671(17) 9_565 ?
S1 Ba1 3.195(2) 3 ?
S1 Ba1 3.2981(14) 13 ?
S1 Ba1 3.2981(14) 13_554 ?
