# Electronic Supplementary Material (ESI) for Materials Advances.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_FeAsSe_52_Pnnm_a
_database_code_depnum_ccdc_archive 'CCDC 1996184'
loop_
_audit_author_name
_audit_author_address
'Xiaoyan Tan'
;George Mason University
United States of America
;
_audit_update_record             
;
2020-04-22 deposited with the CCDC.	2020-07-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'As1.50 Fe Se0.50'
_chemical_formula_weight         207.71

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'
As As 0.0499 2.0058 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_H-M_alt        'P n n m'
_space_group_name_Hall           '-P 2 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, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   5.2135(15)
_cell_length_b                   5.9468(17)
_cell_length_c                   2.9885(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     92.65(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    294(2)
_cell_measurement_reflns_used    708
_cell_measurement_theta_min      5.20
_cell_measurement_theta_max      32.27

_exptl_crystal_description       rod
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    7.445
_exptl_crystal_F_000             185
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.035
_exptl_absorpt_coefficient_mu    43.981
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2679
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_process_details   'Bruker SAINT (SADABS)'
## _exptl_absorpt_special_details    ? 
_diffrn_ambient_temperature      294(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1172
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_av_R_equivalents  0.0200
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_theta_min         5.201
_diffrn_reflns_theta_max         32.009
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             186
_reflns_number_gt                186
_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       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  SHELXL-2014/7
_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)+(0.0340P)²+0.4596P] 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     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.026(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         186
_refine_ls_number_parameters     14
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0245
_refine_ls_wR_factor_ref         0.0584
_refine_ls_wR_factor_gt          0.0584
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_restrained_S_all      1.190
_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
Fe1 Fe 0.500000 0.500000 0.500000 0.0052(3) Uani 1 4 d S T P . .
As2 As 0.31907(9) 0.13693(9) 0.500000 0.0047(2) Uani 0.75 2 d S T P . .
Se2 Se 0.31907(9) 0.13693(9) 0.500000 0.0047(2) Uani 0.25 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
Fe1 0.0039(5) 0.0025(5) 0.0091(5) 0.000 0.000 -0.0006(3)
As2 0.0048(3) 0.0031(3) 0.0063(3) 0.000 0.000 -0.00047(14)
Se2 0.0048(3) 0.0031(3) 0.0063(3) 0.000 0.000 -0.00047(14)

_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
Fe1 Se2 2.3562(8) . ?
Fe1 As2 2.3562(8) 5_666 ?
Fe1 As2 2.3797(6) 7_666 ?
Fe1 As2 2.3797(6) 3 ?
Fe1 As2 2.3797(6) 3_556 ?
Fe1 As2 2.3797(6) 7_665 ?

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
Se2 Fe1 As2 180.0 . 5_666 ?
Se2 Fe1 As2 88.068(16) . 7_666 ?
As2 Fe1 As2 91.932(16) 5_666 7_666 ?
Se2 Fe1 As2 91.932(16) . 3 ?
As2 Fe1 As2 88.068(16) 5_666 3 ?
As2 Fe1 As2 180.0 7_666 3 ?
Se2 Fe1 As2 91.932(16) . 3_556 ?
As2 Fe1 As2 88.068(16) 5_666 3_556 ?
As2 Fe1 As2 102.21(3) 7_666 3_556 ?
As2 Fe1 As2 77.79(2) 3 3_556 ?
Se2 Fe1 As2 88.068(16) . 7_665 ?
As2 Fe1 As2 91.932(16) 5_666 7_665 ?
As2 Fe1 As2 77.79(3) 7_666 7_665 ?
As2 Fe1 As2 102.21(3) 3 7_665 ?
As2 Fe1 As2 180.0 3_556 7_665 ?
Fe1 Se2 Fe1 126.399(17) . 3_545 ?
Fe1 Se2 Fe1 126.399(17) . 3_546 ?
Fe1 Se2 Fe1 77.79(2) 3_545 3_546 ?
Fe1 Se2 As2 107.20(4) . 5_656 ?
Fe1 Se2 As2 107.79(3) 3_545 5_656 ?
Fe1 Se2 As2 107.79(3) 3_546 5_656 ?


_refine_diff_density_max         1.017
_refine_diff_density_min         -1.498
_refine_diff_density_rms         0.356

_shelx_res_file                  
; 
  
TITL FeAsSe_52_Pnnm_a.res in Pnnm 
    FeAsSe_52_Pnnm_a.res 
    created by SHELXL-2016/6 at 12:10:01 on 19-Jul-2018 
REM Old TITL FeAsSe_52_Pnnm in Pnnm 
  
REM SHELXT solution in Pnnm 
REM R1 0.032,  Rweak 0.004,  Alpha 0.027,  Orientation as input 
REM Formula found by SHELXT:  Fe Se2 
  
CELL  0.71073   5.2135   5.9468   2.9885   90.000   90.000   90.000 
ZERR    2.000   0.0015   0.0017   0.0008    0.000    0.000    0.000 
LATT  1 
SYMM -X, -Y, Z 
SYMM 1/2-X, 1/2+Y, 1/2-Z 
SYMM 1/2+X, 1/2-Y, 1/2-Z 
SFAC FE AS SE 
UNIT 2 3 1 
L.S. 22 10 
acta 
conf 
exyz se2 as2 
eadp se2 as2 
BOND 
LIST 4 
FMAP -2 
PLAN 40 
WGHT    0.034000    0.459600 
EXTI    0.026166 
FVAR       0.93807   0.96671   0.37636 
FE1   1    0.500000    0.500000    0.500000    10.25000    0.00387    0.00247 = 
         0.00912    0.00000    0.00000   -0.00058 
AS2   2    0.319070    0.136926    0.500000    10.37500    0.00476    0.00310 = 
         0.00627    0.00000    0.00000   -0.00047 
SE2   3    0.319070    0.136926    0.500000    10.12500    0.00476    0.00310 = 
         0.00627    0.00000    0.00000   -0.00047 
HKLF 4 
  
  
  
  
REM  FeAsSe_52_Pnnm_a.res in Pnnm 
REM R1 =  0.0245 for     186 Fo > 4sig(Fo)  and  0.0245 for all     186 data 
REM     14 parameters refined using      0 restraints 
  
END 
  
WGHT      0.0341      0.4614 
  
REM Highest difference peak  1.017,  deepest hole -1.498,  1-sigma level  0.356 
Q1    1   0.4180  0.0432  0.5000  10.50000  0.05   -1.50 
Q2    1   0.2361  0.0350  0.5000  10.50000  0.05   -1.39 
Q3    1   0.2067  0.3441  0.5000  10.50000  0.05   -1.24 
Q4    1   0.5000  0.5000  0.0000  10.25000  0.05   -1.22 
Q5    1   0.1640 -0.0908  0.5000  10.50000  0.05   -1.17 
Q6    1   0.4160  0.3990  0.5000  10.50000  0.05   -1.17 
Q7    1   0.1954  0.2238  0.5000  10.50000  0.05   -1.02 
Q8    1   0.4861  0.1421  0.5000  10.50000  0.05    1.02 
Q9    1   0.3528  0.0239  0.0000  10.50000  0.05   -0.92 
Q10   1   0.5137  0.0736  0.0000  10.50000  0.05   -0.91 
Q11   1   0.3606  0.1976  0.2453  11.00000  0.05    0.88 
Q12   1   0.1938  0.0636  0.2273  11.00000  0.05    0.85 
Q13   1   0.3286  0.7400  0.5000  10.50000  0.05   -0.84 
Q14   1   0.2357  0.1652  0.2035  11.00000  0.05    0.82 
Q15   1   0.4576  0.2923  0.5000  10.50000  0.05    0.81 
Q16   1   0.5000  0.0000  0.3894  10.50000  0.05    0.76 
Q17   1   0.2625  0.3029  0.0663  11.00000  0.05    0.72 
Q18   1   0.5056  0.1541  0.6975  11.00000  0.05    0.72 
Q19   1   0.3823  0.1012  0.1996  11.00000  0.05    0.72 
Q20   1   0.4631  0.2734  0.1299  11.00000  0.05   -0.70 
Q21   1   0.5000  0.5000  0.2456  10.50000  0.05    0.69 
Q22   1   0.1886  0.1334  0.5000  10.50000  0.05    0.69 
Q23   1   0.4345 -0.0532  0.5000  10.50000  0.05   -0.68 
Q24   1   0.3407  0.2933  0.3858  11.00000  0.05   -0.67 
Q25   1   0.5000  0.0000  0.1768  10.50000  0.05   -0.65 
Q26   1   0.4250  0.6032  0.2380  11.00000  0.05    0.65 
Q27   1   0.4086  0.2094  0.4369  11.00000  0.05   -0.62 
Q28   1   0.3681  0.5147  0.5000  10.50000  0.05    0.61 
Q29   1   0.3122  0.3879  0.4014  11.00000  0.05    0.58 
Q30   1   0.4329  0.1389  0.0000  10.50000  0.05   -0.54 
Q31   1   0.3345 -0.0508  0.5000  10.50000  0.05    0.52 
Q32   1   0.6074  0.1540  0.6330  11.00000  0.05    0.50 
Q33   1   0.3019  0.5800  0.5000  10.50000  0.05   -0.48 
Q34   1   0.5479  0.2207  0.5000  10.50000  0.05   -0.48 
Q35   1   0.1619  0.4351  0.5000  10.50000  0.05    0.41 
Q36   1   0.3174  0.2231  0.5000  10.50000  0.05    0.41 
Q37   1   0.1228  0.0076  0.5000  10.50000  0.05    0.36 
Q38   1   0.1428  0.2598  0.3466  11.00000  0.05    0.36 
Q39   1   0.2747  0.4375  0.2423  11.00000  0.05   -0.34 
Q40   1   0.4174  0.3471  0.0000  10.50000  0.05    0.34 
;
_shelx_res_checksum              47925
