# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_exp_4551
_database_code_depnum_ccdc_archive 'CCDC 1051630'
_audit_update_record             
;
2015-02-28 deposited with the CCDC.
2015-04-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'H Fe1.15 Li0.85 O S'
_chemical_formula_weight         119.1912

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P 4/n m m'

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

_cell_length_a                   3.6886(3)
_cell_length_b                   3.6886(3)
_cell_length_c                   8.9149(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     121.29(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    184
_cell_measurement_theta_min      5.9240
_cell_measurement_theta_max      29.1670

_exptl_crystal_description       Plate
_exptl_crystal_colour            Black
_exptl_crystal_size_max          0.1039
_exptl_crystal_size_mid          0.1039
_exptl_crystal_size_min          0.0389
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.258
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             80
_exptl_absorpt_coefficient_mu    7.530
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.476
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            254
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         4.57
_diffrn_reflns_theta_max         28.87
_reflns_number_total             121
_reflns_number_gt                103
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0648P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.10(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         121
_refine_ls_number_parameters     15
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0303
_refine_ls_wR_factor_ref         0.0815
_refine_ls_wR_factor_gt          0.0813
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.7500 0.2500 0.5000 0.0096(6) Uani 1 8 d S . .
S2 S 0.2500 0.2500 0.64430(13) 0.0105(7) Uani 1 8 d S . .
O3 O 0.2500 0.2500 0.0798(5) 0.0183(11) Uani 1 8 d S . .
Fe2 Fe 0.2500 -0.2500 0.0000 0.039(4) Uani 0.146(13) 8 d SP . .
Li2 Li 0.2500 -0.2500 0.0000 0.039(4) Uani 0.854(13) 8 d SP . .
H4 H 0.2500 0.2500 0.153(9) 0.10(6) Uiso 1 8 d S . .

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 0.0066(6) 0.0066(6) 0.0157(7) 0.000 0.000 0.000
S2 0.0084(8) 0.0084(8) 0.0146(9) 0.000 0.000 0.000
O3 0.0157(16) 0.0157(16) 0.023(3) 0.000 0.000 0.000
Fe2 0.015(3) 0.015(3) 0.085(7) 0.000 0.000 0.000
Li2 0.015(3) 0.015(3) 0.085(7) 0.000 0.000 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
Fe1 S2 2.2486(7) 9_656 ?
Fe1 S2 2.2486(7) 1_655 ?
Fe1 S2 2.2486(7) 9_666 ?
Fe1 S2 2.2486(7) . ?
Fe1 Fe1 2.6082(2) 9_656 ?
Fe1 Fe1 2.6082(2) 9_766 ?
Fe1 Fe1 2.6082(2) 9_756 ?
Fe1 Fe1 2.6082(2) 9_666 ?
S2 Fe1 2.2486(7) 9_656 ?
S2 Fe1 2.2486(7) 1_455 ?
S2 Fe1 2.2486(7) 9_666 ?
O3 Li2 1.9769(16) 9 ?
O3 Fe2 1.9769(16) . ?
O3 Fe2 1.9769(16) 9 ?
O3 Li2 1.9769(16) 9_655 ?
O3 Fe2 1.9769(16) 9_655 ?
O3 Li2 1.9769(16) 1_565 ?
O3 Fe2 1.9769(16) 1_565 ?
Fe2 O3 1.9769(16) 9 ?
Fe2 O3 1.9769(16) 9_655 ?
Fe2 O3 1.9769(16) 1_545 ?
Fe2 Li2 2.6082(2) 9_655 ?
Fe2 Fe2 2.6082(2) 9_545 ?
Fe2 Li2 2.6082(2) 9_545 ?
Fe2 Fe2 2.6082(2) 9_655 ?
Fe2 Fe2 2.6082(2) 9_645 ?
Fe2 Fe2 2.6082(2) 9 ?
Fe2 Li2 2.6082(2) 9_645 ?
Fe2 Li2 2.6082(2) 9 ?

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
S2 Fe1 S2 109.10(2) 9_656 1_655 ?
S2 Fe1 S2 110.21(5) 9_656 9_666 ?
S2 Fe1 S2 109.10(2) 1_655 9_666 ?
S2 Fe1 S2 109.10(2) 9_656 . ?
S2 Fe1 S2 110.21(5) 1_655 . ?
S2 Fe1 S2 109.10(2) 9_666 . ?
S2 Fe1 Fe1 54.552(12) 9_656 9_656 ?
S2 Fe1 Fe1 125.448(12) 1_655 9_656 ?
S2 Fe1 Fe1 125.448(12) 9_666 9_656 ?
S2 Fe1 Fe1 54.552(12) . 9_656 ?
S2 Fe1 Fe1 125.448(12) 9_656 9_766 ?
S2 Fe1 Fe1 54.552(12) 1_655 9_766 ?
S2 Fe1 Fe1 54.552(12) 9_666 9_766 ?
S2 Fe1 Fe1 125.448(12) . 9_766 ?
Fe1 Fe1 Fe1 180.0 9_656 9_766 ?
S2 Fe1 Fe1 54.552(12) 9_656 9_756 ?
S2 Fe1 Fe1 54.552(12) 1_655 9_756 ?
S2 Fe1 Fe1 125.448(12) 9_666 9_756 ?
S2 Fe1 Fe1 125.448(12) . 9_756 ?
Fe1 Fe1 Fe1 90.0 9_656 9_756 ?
Fe1 Fe1 Fe1 90.0 9_766 9_756 ?
S2 Fe1 Fe1 125.448(12) 9_656 9_666 ?
S2 Fe1 Fe1 125.448(12) 1_655 9_666 ?
S2 Fe1 Fe1 54.552(12) 9_666 9_666 ?
S2 Fe1 Fe1 54.552(12) . 9_666 ?
Fe1 Fe1 Fe1 90.0 9_656 9_666 ?
Fe1 Fe1 Fe1 90.0 9_766 9_666 ?
Fe1 Fe1 Fe1 180.0 9_756 9_666 ?
Fe1 S2 Fe1 70.90(2) 9_656 1_455 ?
Fe1 S2 Fe1 110.21(5) 9_656 9_666 ?
Fe1 S2 Fe1 70.90(2) 1_455 9_666 ?
Fe1 S2 Fe1 70.90(2) 9_656 . ?
Fe1 S2 Fe1 110.21(5) 1_455 . ?
Fe1 S2 Fe1 70.90(2) 9_666 . ?
Li2 O3 Fe2 82.55(8) 9 . ?
Li2 O3 Fe2 0.0 9 9 ?
Fe2 O3 Fe2 82.55(8) . 9 ?
Li2 O3 Li2 137.8(2) 9 9_655 ?
Fe2 O3 Li2 82.55(8) . 9_655 ?
Fe2 O3 Li2 137.8(2) 9 9_655 ?
Li2 O3 Fe2 137.8(2) 9 9_655 ?
Fe2 O3 Fe2 82.55(8) . 9_655 ?
Fe2 O3 Fe2 137.8(2) 9 9_655 ?
Li2 O3 Fe2 0.0 9_655 9_655 ?
Li2 O3 Li2 82.55(8) 9 1_565 ?
Fe2 O3 Li2 137.8(2) . 1_565 ?
Fe2 O3 Li2 82.55(8) 9 1_565 ?
Li2 O3 Li2 82.55(8) 9_655 1_565 ?
Fe2 O3 Li2 82.55(8) 9_655 1_565 ?
Li2 O3 Fe2 82.55(8) 9 1_565 ?
Fe2 O3 Fe2 137.8(2) . 1_565 ?
Fe2 O3 Fe2 82.55(8) 9 1_565 ?
Li2 O3 Fe2 82.55(8) 9_655 1_565 ?
Fe2 O3 Fe2 82.55(8) 9_655 1_565 ?
Li2 O3 Fe2 0.0 1_565 1_565 ?
O3 Fe2 O3 97.45(8) 9 . ?
O3 Fe2 O3 137.8(2) 9 9_655 ?
O3 Fe2 O3 97.45(8) . 9_655 ?
O3 Fe2 O3 97.45(8) 9 1_545 ?
O3 Fe2 O3 137.8(2) . 1_545 ?
O3 Fe2 O3 97.45(8) 9_655 1_545 ?
O3 Fe2 Li2 131.28(4) 9 9_655 ?
O3 Fe2 Li2 48.72(4) . 9_655 ?
O3 Fe2 Li2 48.72(4) 9_655 9_655 ?
O3 Fe2 Li2 131.28(4) 1_545 9_655 ?
O3 Fe2 Fe2 48.72(4) 9 9_545 ?
O3 Fe2 Fe2 131.28(4) . 9_545 ?
O3 Fe2 Fe2 131.28(4) 9_655 9_545 ?
O3 Fe2 Fe2 48.72(4) 1_545 9_545 ?
Li2 Fe2 Fe2 180.0 9_655 9_545 ?
O3 Fe2 Li2 48.72(4) 9 9_545 ?
O3 Fe2 Li2 131.28(4) . 9_545 ?
O3 Fe2 Li2 131.28(4) 9_655 9_545 ?
O3 Fe2 Li2 48.72(4) 1_545 9_545 ?
Li2 Fe2 Li2 180.0 9_655 9_545 ?
Fe2 Fe2 Li2 0.0 9_545 9_545 ?
O3 Fe2 Fe2 131.28(4) 9 9_655 ?
O3 Fe2 Fe2 48.72(4) . 9_655 ?
O3 Fe2 Fe2 48.72(4) 9_655 9_655 ?
O3 Fe2 Fe2 131.28(4) 1_545 9_655 ?
Li2 Fe2 Fe2 0.0 9_655 9_655 ?
Fe2 Fe2 Fe2 180.0 9_545 9_655 ?
Li2 Fe2 Fe2 180.0 9_545 9_655 ?
O3 Fe2 Fe2 131.28(4) 9 9_645 ?
O3 Fe2 Fe2 131.28(4) . 9_645 ?
O3 Fe2 Fe2 48.72(4) 9_655 9_645 ?
O3 Fe2 Fe2 48.72(4) 1_545 9_645 ?
Li2 Fe2 Fe2 90.0 9_655 9_645 ?
Fe2 Fe2 Fe2 90.0 9_545 9_645 ?
Li2 Fe2 Fe2 90.0 9_545 9_645 ?
Fe2 Fe2 Fe2 90.0 9_655 9_645 ?
O3 Fe2 Fe2 48.72(4) 9 9 ?
O3 Fe2 Fe2 48.72(4) . 9 ?
O3 Fe2 Fe2 131.28(4) 9_655 9 ?
O3 Fe2 Fe2 131.28(4) 1_545 9 ?
Li2 Fe2 Fe2 90.0 9_655 9 ?
Fe2 Fe2 Fe2 90.0 9_545 9 ?
Li2 Fe2 Fe2 90.0 9_545 9 ?
Fe2 Fe2 Fe2 90.0 9_655 9 ?
Fe2 Fe2 Fe2 180.0 9_645 9 ?
O3 Fe2 Li2 131.28(4) 9 9_645 ?
O3 Fe2 Li2 131.28(4) . 9_645 ?
O3 Fe2 Li2 48.72(4) 9_655 9_645 ?
O3 Fe2 Li2 48.72(4) 1_545 9_645 ?
Li2 Fe2 Li2 90.0 9_655 9_645 ?
Fe2 Fe2 Li2 90.0 9_545 9_645 ?
Li2 Fe2 Li2 90.0 9_545 9_645 ?
Fe2 Fe2 Li2 90.0 9_655 9_645 ?
Fe2 Fe2 Li2 0.0 9_645 9_645 ?
Fe2 Fe2 Li2 180.0 9 9_645 ?
O3 Fe2 Li2 48.72(4) 9 9 ?
O3 Fe2 Li2 48.72(4) . 9 ?
O3 Fe2 Li2 131.28(4) 9_655 9 ?
O3 Fe2 Li2 131.28(4) 1_545 9 ?
Li2 Fe2 Li2 90.0 9_655 9 ?
Fe2 Fe2 Li2 90.0 9_545 9 ?
Li2 Fe2 Li2 90.0 9_545 9 ?
Fe2 Fe2 Li2 90.0 9_655 9 ?
Fe2 Fe2 Li2 180.0 9_645 9 ?
Fe2 Fe2 Li2 0.0 9 9 ?
Li2 Fe2 Li2 180.0 9_645 9 ?


_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        24.96
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.886
_refine_diff_density_rms         0.169
