# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_sad
_database_code_depnum_ccdc_archive 'CCDC 1537571'
_audit_update_record             
;
2017-03-12 deposited with the CCDC.
2017-05-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ba Fe1.95 Se3'
_chemical_formula_weight         483.13

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   11.936(2)
_cell_length_b                   5.4322(10)
_cell_length_c                   9.1679(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     594.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1681
_cell_measurement_theta_min      2.80
_cell_measurement_theta_max      28.81

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    5.399
_exptl_crystal_F_000             835
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    29.464
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2889
_diffrn_reflns_av_unetI/netI     0.0717
_diffrn_reflns_av_R_equivalents  0.1261
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.802
_diffrn_reflns_theta_max         24.990
_diffrn_reflns_theta_full        24.990
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 0.978
_reflns_number_total             570
_reflns_number_gt                555
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+24.2635P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         570
_refine_ls_number_parameters     34
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0433
_refine_ls_wR_factor_ref         0.1072
_refine_ls_wR_factor_gt          0.1063
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Se1 Se 0.35873(14) -0.2500 0.27118(19) 0.0197(5) Uani 1 2 d S T P . .
Se2 Se 0.37214(14) 0.2500 -0.00868(17) 0.0165(4) Uani 1 2 d S T P . .
Se3 Se 0.60123(15) 0.2500 0.31325(19) 0.0227(5) Uani 1 2 d S T P . .
Fe1 Fe 0.49439(13) -0.0004(3) 0.14733(18) 0.0130(5) Uani 0.975 1 d . . P . .
Ba1 Ba 0.31518(9) 0.2500 0.48056(12) 0.0244(4) Uani 1 2 d S T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Se1 0.0225(10) 0.0158(8) 0.0208(9) 0.000 0.0085(7) 0.000
Se2 0.0167(10) 0.0145(8) 0.0183(8) 0.000 0.0008(6) 0.000
Se3 0.0270(10) 0.0170(8) 0.0240(9) 0.000 -0.0128(7) 0.000
Fe1 0.0106(9) 0.0148(9) 0.0135(8) -0.0002(7) 0.0003(6) 0.0008(6)
Ba1 0.0278(7) 0.0184(6) 0.0270(6) 0.000 0.0065(5) 0.000

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Se1 Fe1 2.398(2) . ?
Se1 Fe1 2.398(2) 7 ?
Se1 Ba1 3.3663(12) . ?
Se1 Ba1 3.3663(12) 1_545 ?
Se1 Ba1 3.378(2) 2_554 ?
Se2 Fe1 2.448(2) 3_655 ?
Se2 Fe1 2.448(2) 5_655 ?
Se2 Fe1 2.455(2) 7_565 ?
Se2 Fe1 2.455(2) . ?
Se2 Ba1 3.5194(14) 2_554 ?
Se2 Ba1 3.5194(14) 2_564 ?
Se3 Fe1 2.406(2) . ?
Se3 Fe1 2.406(2) 7_565 ?
Se3 Ba1 3.4563(13) 5_666 ?
Se3 Ba1 3.4563(13) 5_656 ?
Se3 Ba1 3.712(2) 6_656 ?
Se3 Ba1 3.743(2) . ?
Fe1 Se2 2.448(2) 5_655 ?
Fe1 Fe1 2.705(3) 5_655 ?
Fe1 Fe1 2.712(3) 7 ?
Fe1 Fe1 2.721(3) 7_565 ?
Ba1 Se1 3.3663(12) 1_565 ?
Ba1 Se1 3.378(2) 2 ?
Ba1 Se3 3.4563(13) 5_666 ?
Ba1 Se3 3.4563(13) 5_656 ?
Ba1 Se2 3.5194(14) 2 ?
Ba1 Se2 3.5194(14) 2_565 ?
Ba1 Se3 3.712(2) 6_556 ?

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
Fe1 Se1 Fe1 68.86(9) . 7 ?
Fe1 Se1 Ba1 85.30(4) . . ?
Fe1 Se1 Ba1 146.15(7) 7 . ?
Fe1 Se1 Ba1 146.15(7) . 1_545 ?
Fe1 Se1 Ba1 85.30(4) 7 1_545 ?
Ba1 Se1 Ba1 107.58(5) . 1_545 ?
Fe1 Se1 Ba1 92.38(7) . 2_554 ?
Fe1 Se1 Ba1 92.38(7) 7 2_554 ?
Ba1 Se1 Ba1 110.79(4) . 2_554 ?
Ba1 Se1 Ba1 110.79(4) 1_545 2_554 ?
Fe1 Se2 Fe1 67.27(8) 3_655 5_655 ?
Fe1 Se2 Fe1 66.97(7) 3_655 7_565 ?
Fe1 Se2 Fe1 102.87(7) 5_655 7_565 ?
Fe1 Se2 Fe1 102.87(7) 3_655 . ?
Fe1 Se2 Fe1 66.97(7) 5_655 . ?
Fe1 Se2 Fe1 67.31(8) 7_565 . ?
Fe1 Se2 Ba1 145.73(7) 3_655 2_554 ?
Fe1 Se2 Ba1 88.36(4) 5_655 2_554 ?
Fe1 Se2 Ba1 145.25(7) 7_565 2_554 ?
Fe1 Se2 Ba1 88.07(4) . 2_554 ?
Fe1 Se2 Ba1 88.36(4) 3_655 2_564 ?
Fe1 Se2 Ba1 145.73(7) 5_655 2_564 ?
Fe1 Se2 Ba1 88.07(4) 7_565 2_564 ?
Fe1 Se2 Ba1 145.25(7) . 2_564 ?
Ba1 Se2 Ba1 101.02(5) 2_554 2_564 ?
Fe1 Se3 Fe1 68.85(9) . 7_565 ?
Fe1 Se3 Ba1 160.55(6) . 5_666 ?
Fe1 Se3 Ba1 93.12(4) 7_565 5_666 ?
Fe1 Se3 Ba1 93.12(4) . 5_656 ?
Fe1 Se3 Ba1 160.55(6) 7_565 5_656 ?
Ba1 Se3 Ba1 103.60(5) 5_666 5_656 ?
Fe1 Se3 Ba1 84.60(6) . 6_656 ?
Fe1 Se3 Ba1 84.60(6) 7_565 6_656 ?
Ba1 Se3 Ba1 101.44(4) 5_666 6_656 ?
Ba1 Se3 Ba1 101.44(4) 5_656 6_656 ?
Fe1 Se3 Ba1 77.04(6) . . ?
Fe1 Se3 Ba1 77.04(6) 7_565 . ?
Ba1 Se3 Ba1 92.25(4) 5_666 . ?
Ba1 Se3 Ba1 92.25(4) 5_656 . ?
Ba1 Se3 Ba1 157.66(5) 6_656 . ?
Se1 Fe1 Se3 112.22(9) . . ?
Se1 Fe1 Se2 111.85(7) . 5_655 ?
Se3 Fe1 Se2 107.25(8) . 5_655 ?
Se1 Fe1 Se2 100.83(8) . . ?
Se3 Fe1 Se2 111.72(7) . . ?
Se2 Fe1 Se2 113.03(7) 5_655 . ?
Se1 Fe1 Fe1 120.49(10) . 5_655 ?
Se3 Fe1 Fe1 127.17(10) . 5_655 ?
Se2 Fe1 Fe1 56.64(6) 5_655 5_655 ?
Se2 Fe1 Fe1 56.39(6) . 5_655 ?
Se1 Fe1 Fe1 55.57(4) . 7 ?
Se3 Fe1 Fe1 124.42(4) . 7 ?
Se2 Fe1 Fe1 56.37(4) 5_655 7 ?
Se2 Fe1 Fe1 123.65(4) . 7 ?
Fe1 Fe1 Fe1 90.10(6) 5_655 7 ?
Se1 Fe1 Fe1 124.43(4) . 7_565 ?
Se3 Fe1 Fe1 55.58(4) . 7_565 ?
Se2 Fe1 Fe1 123.63(4) 5_655 7_565 ?
Se2 Fe1 Fe1 56.35(4) . 7_565 ?
Fe1 Fe1 Fe1 89.90(6) 5_655 7_565 ?
Fe1 Fe1 Fe1 180.00(14) 7 7_565 ?
Se1 Ba1 Se1 107.58(5) 1_565 . ?
Se1 Ba1 Se1 123.00(2) 1_565 2 ?
Se1 Ba1 Se1 123.00(2) . 2 ?
Se1 Ba1 Se3 68.48(4) 1_565 5_666 ?
Se1 Ba1 Se3 154.34(6) . 5_666 ?
Se1 Ba1 Se3 75.28(4) 2 5_666 ?
Se1 Ba1 Se3 154.34(6) 1_565 5_656 ?
Se1 Ba1 Se3 68.48(4) . 5_656 ?
Se1 Ba1 Se3 75.28(4) 2 5_656 ?
Se3 Ba1 Se3 103.60(5) 5_666 5_656 ?
Se1 Ba1 Se2 137.46(5) 1_565 2 ?
Se1 Ba1 Se2 59.43(4) . 2 ?
Se1 Ba1 Se2 65.64(3) 2 2 ?
Se3 Ba1 Se2 140.76(5) 5_666 2 ?
Se3 Ba1 Se2 64.00(4) 5_656 2 ?
Se1 Ba1 Se2 59.43(4) 1_565 2_565 ?
Se1 Ba1 Se2 137.46(5) . 2_565 ?
Se1 Ba1 Se2 65.64(3) 2 2_565 ?
Se3 Ba1 Se2 64.00(4) 5_666 2_565 ?
Se3 Ba1 Se2 140.76(5) 5_656 2_565 ?
Se2 Ba1 Se2 101.02(5) 2 2_565 ?
Se1 Ba1 Se3 72.09(4) 1_565 6_556 ?
Se1 Ba1 Se3 72.09(4) . 6_556 ?
Se1 Ba1 Se3 98.61(5) 2 6_556 ?
Se3 Ba1 Se3 126.55(2) 5_666 6_556 ?
Se3 Ba1 Se3 126.55(2) 5_656 6_556 ?
Se2 Ba1 Se3 65.37(3) 2 6_556 ?
Se2 Ba1 Se3 65.37(3) 2_565 6_556 ?
Se1 Ba1 Se3 68.01(4) 1_565 . ?
Se1 Ba1 Se3 68.01(4) . . ?
Se1 Ba1 Se3 152.11(5) 2 . ?
Se3 Ba1 Se3 87.75(4) 5_666 . ?
Se3 Ba1 Se3 87.75(4) 5_656 . ?
Se2 Ba1 Se3 126.23(3) 2 . ?
Se2 Ba1 Se3 126.23(3) 2_565 . ?
Se3 Ba1 Se3 109.28(3) 6_556 . ?

_refine_diff_density_max         1.535
_refine_diff_density_min         -1.886
_refine_diff_density_rms         0.347

_shelx_res_file                  
;

    sad.res created by SHELXL-2014/7


TITL sad in Pnma
CELL 0.71073  11.9358   5.4322   9.1679  90.000  90.000  90.000
ZERR    4.00   0.0024   0.0010   0.0018   0.000   0.000   0.000
LATT  1
SYMM 0.5-X, -Y, 0.5+Z
SYMM -X, 0.5+Y, -Z
SYMM 0.5+X, 0.5-Y, 0.5-Z
SFAC FE SE BA
UNIT 7.8 12 4
TEMP 23.000
omit  8   0   5
omit  1   5   4
omit  8   0   9
omit  10   5   3
omit  8   4   5
omit  1   1   4
omit  10   1   3
omit  13   2   1
omit  9   0   2
omit  2   0   0
omit  1   0  10
omit  6   1   7
omit  8   2   5
omit 0 50
L.S. 15
BOND
acta
FMAP 2
PLAN -20

WGHT    0.000000   24.263500
FVAR       0.06320
SE1   2    0.358728   -0.250000    0.271184    10.50000    0.02254    0.01581 =
         0.02078    0.00000    0.00849    0.00000
SE2   2    0.372141    0.250000   -0.008680    10.50000    0.01666    0.01446 =
         0.01827    0.00000    0.00078    0.00000
SE3   2    0.601228    0.250000    0.313255    10.50000    0.02701    0.01703 =
         0.02401    0.00000   -0.01279    0.00000
FE1   1    0.494393   -0.000421    0.147331    10.97500    0.01064    0.01485 =
         0.01351   -0.00025    0.00029    0.00080
BA1   3    0.315183    0.250000    0.480558    10.50000    0.02779    0.01839 =
         0.02699    0.00000    0.00651    0.00000
HKLF 4

REM  sad in Pnma
REM R1 =  0.0433 for     555 Fo > 4sig(Fo)  and  0.0452 for all     570 data
REM     34 parameters refined using      0 restraints

END

WGHT      0.0000     14.1859

REM Highest difference peak  1.535,  deepest hole -1.886,  1-sigma level  0.347
Q1    1   0.3913 -0.2500  0.5666  10.50000  0.05    1.53
Q2    1   0.3581 -0.2500  0.1706  10.50000  0.05    1.47
Q3    1   0.3853  0.2500 -0.1445  10.50000  0.05    1.32
Q4    1   0.3248 -0.7500  0.3760  10.50000  0.05    1.30
Q5    1   0.4891 -0.0872  0.2447  11.00000  0.05    1.20
Q6    1   0.6964  0.2500  0.1908  10.50000  0.05    1.19
Q7    1   0.5972  0.1785  0.2150  11.00000  0.05    1.11
Q8    1   0.4524 -0.2500  0.1815  10.50000  0.05    1.08
Q9    1   0.4012  0.0683  0.4695  11.00000  0.05    1.03
Q10   1   0.5065  0.2500  0.1929  10.50000  0.05    0.99
Q11   1   0.3785 -0.2500  0.4015  10.50000  0.05    0.98
Q12   1   0.4979  0.0739  0.0204  11.00000  0.05    0.96
Q13   1   0.5026 -0.0592  0.4435  11.00000  0.05    0.95
Q14   1   0.4010 -0.0813  0.2440  11.00000  0.05    0.88
Q15   1   0.3723  0.2500  0.1072  10.50000  0.05    0.86
Q16   1   0.6657 -0.1158  0.4368  11.00000  0.05    0.86
Q17   1   0.4774 -0.0674  0.0403  11.00000  0.05    0.85
Q18   1   0.2954 -0.0654  0.2119  11.00000  0.05    0.84
Q19   1   0.3986  0.1204  0.0598  11.00000  0.05    0.82
Q20   1   0.1806 -0.1551  0.0865  11.00000  0.05    0.81
;
_shelx_res_checksum              10473
