# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# 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_19CGC005CT300K
_database_code_depnum_ccdc_archive 'CCDC 2000618'
loop_
_audit_author_name
_audit_author_address
'Antonio L. Llamas-Saiz'
;Universidade de Santiago de Compostela
Spain
;
_audit_update_record             
;
2020-05-02 deposited with the CCDC.	2020-08-29 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            '[TMS][FeCl4] - T300K'
_chemical_formula_moiety         'C3 H9 S, Cl4 Fe'
_chemical_formula_sum            'C3 H9 Cl4 Fe S'
_chemical_formula_iupac          ?
_chemical_formula_weight         274.81

_chemical_melting_point          ?

_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
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                   12.707(4)
_cell_length_b                   7.900(2)
_cell_length_c                   11.551(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1159.6(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3855
_cell_measurement_theta_min      2.3828
_cell_measurement_theta_max      24.6072
_cell_measurement_temperature    300.(2)

_exptl_crystal_description       block
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_size_max          0.171
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.056
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             548

_exptl_absorpt_coefficient_mu    2.337
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_T_max  0.88

_exptl_special_details           
;
;

_diffrn_ambient_temperature      300.(2)

_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS 3.0'

_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'multilayer mirror'

_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON-III C14'
_diffrn_measurement_method       'φ or ω oscillation scans'

_diffrn_detector_area_resol_mean 7.3910

_diffrn_reflns_number            11340
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_theta_min         2.38
_diffrn_reflns_theta_max         27.13
_diffrn_reflns_theta_full        27.13
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14

_refine_special_details          
;
;

_reflns_number_total             1372
_reflns_number_gt                889
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0484
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1493
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.017
_refine_ls_number_reflns         1372
_refine_ls_number_parameters     83
_refine_ls_number_restraints     94
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0608P)²+1.1959P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.262
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_computing_data_collection       'Bruker APEX3 software'
_computing_cell_refinement       'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'ORTEP 2014.1 (Farrugia, 2012)'
_computing_publication_material  'IUCr Journals printCIF'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe1 0.49635(6) 0.75 0.27995(8) 0.0785(4) Uani d T P S 1.0 . .
Cl Cl1 0.44390(12) 0.5232(2) 0.18915(16) 0.1254(6) Uani d . . . 1.0 . .
Cl Cl2 0.66854(13) 0.75 0.27937(18) 0.1021(6) Uani d T P S 1.0 . .
Cl Cl3 0.4407(2) 0.75 0.45682(19) 0.1372(9) Uani d T P S 1.0 . .
S S1^a 0.1645(2) 0.25 0.3948(2) 0.0897(10) Uani d TU P DS 0.652(5) A 1
C C1^a 0.2216(10) 0.4215(17) 0.4416(14) 0.122(4) Uani d U P D 0.652(5) A 1
H H1A^a 0.295975 0.414156 0.427899 0.183 Uiso calc U P DR 0.652(5) A 1
H H1B^a 0.208887 0.433586 0.523105 0.183 Uiso calc U P DR 0.652(5) A 1
H H1C^a 0.193564 0.517783 0.401371 0.183 Uiso calc U P DR 0.652(5) A 1
C C2^a 0.1970(14) 0.25 0.2325(10) 0.093(4) Uani d TU P DS 0.652(5) A 1
H H2A^a 0.165(3) 0.3496(13) 0.203(4) 0.14 Uiso d U P D 0.652(5) A 1
H H2B^a 0.270(2) 0.25 0.227(4) 0.14 Uiso d U P DS 0.652(5) A 1
S S1B^b 0.2764(5) 0.25 0.3667(5) 0.110(2) Uani d TU P DS 0.348(5) A 2
C C1B^b 0.2607(19) 0.426(3) 0.434(2) 0.112(5) Uani d U P D 0.348(5) A 2
H H1D^b 0.290074 0.516786 0.38943 0.169 Uiso calc U P R 0.348(5) A 2
H H1E^b 0.295746 0.420633 0.507986 0.169 Uiso calc U P R 0.348(5) A 2
H H1F^b 0.187003 0.446303 0.446339 0.169 Uiso calc U P R 0.348(5) A 2
C C2B^b 0.169(3) 0.25 0.250(2) 0.097(6) Uani d TU P DS 0.348(5) A 2
H H2D^b 0.180(5) 0.3496(13) 0.206(3) 0.146 Uiso d U P D 0.348(5) A 2
H H2E^b 0.105(3) 0.25 0.290(5) 0.146 Uiso d U P DS 0.348(5) A 2


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 Cl3 . 2.162(2) ?
Fe1 Cl1 . 2.1808(16) ?
Fe1 Cl1_$1 7_575 2.1809(16) ?
Fe1 Cl2 . 2.188(2) ?
S1^a C1^a_$2 7_565 1.629(10) ?
S1^a C1^a . 1.629(10) ?
S1^a C2^a . 1.920(13) ?
C1^a H1A^a . 0.96 ?
C1^a H1B^a . 0.96 ?
C1^a H1C^a . 0.96 ?
C2^a H2A^a . 0.947(16) ?
C2^a H2B^a . 0.934(19) ?
C2^a H2A^a_$2 7_565 0.947(16) ?
C2^a H2D^b_$2 7_565 0.87(2) ?
S1B^b C1B^b_$2 7_565 1.609(15) ?
S1B^b C1B^b . 1.609(15) ?
S1B^b C2B^b . 1.917(18) ?
C1B^b H1D^b . 0.96 ?
C1B^b H1E^b . 0.96 ?
C1B^b H1F^b . 0.96 ?
C2B^b H2D^b . 0.945(16) ?
C2B^b H2E^b . 0.94(2) ?
C2B^b H2D^b_$2 7_565 0.945(16) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl3 Fe1 Cl1 . . 110.77(7) ?
Cl3 Fe1 Cl1_$1 . 7_575 110.77(7) ?
Cl1 Fe1 Cl1_$1 . 7_575 110.52(11) ?
Cl3 Fe1 Cl2 . . 109.25(10) ?
Cl1 Fe1 Cl2 . . 107.71(6) ?
Cl1 Fe1 Cl2 7_575 . 107.71(6) ?
C1^a S1^a C1^a 7_565 . 112.6(12) ?
C1^a S1^a C2^a 7_565 . 103.2(6) ?
C1^a S1^a C2^a . . 103.2(6) ?
S1^a C1^a H1A^a . . 109.5 ?
S1^a C1^a H1B^a . . 109.5 ?
H1A^a C1^a H1B^a . . 109.5 ?
S1^a C1^a H1C^a . . 109.5 ?
H1A^a C1^a H1C^a . . 109.5 ?
H1B^a C1^a H1C^a . . 109.5 ?
S1^a C2^a H2A^a . . 105.(3) ?
S1^a C2^a H2B^a . . 106.(3) ?
H2A^a C2^a H2B^a . . 114.(3) ?
S1^a C2^a H2A^a_$2 . 7_565 105.(3) ?
H2A^a C2^a H2A^a_$2 . 7_565 112.(3) ?
H2B^a C2^a H2A^a_$2 . 7_565 114.(3) ?
S1^a C2^a H2D^b_$2 . 7_565 107.(3) ?
H2A^a C2^a H2D^b_$2 . 7_565 122.(4) ?
H2B^a C2^a H2D^b_$2 . 7_565 103.(4) ?
C1B^b S1B^b C1B^b 7_565 . 120.(2) ?
C1B^b S1B^b C2B^b 7_565 . 104.7(10) ?
C1B^b S1B^b C2B^b . . 104.7(10) ?
S1B^b C1B^b H1D^b . . 109.5 ?
S1B^b C1B^b H1E^b . . 109.5 ?
H1D^b C1B^b H1E^b . . 109.5 ?
S1B^b C1B^b H1F^b . . 109.5 ?
H1D^b C1B^b H1F^b . . 109.5 ?
H1E^b C1B^b H1F^b . . 109.5 ?
S1B^b C2B^b H2D^b . . 105.(3) ?
S1B^b C2B^b H2E^b . . 106.(3) ?
H2D^b C2B^b H2E^b . . 113.(3) ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C1^a H1B^a Cl1 2_565 0.96 2.75 3.576(15) 144.6 ?
C1^a H1C^a Cl2 6_556 0.96 2.8 3.702(18) 157.4 ?
C1B^b H1D^b Cl3 . 0.96 2.77 3.44(2) 127.8 ?
C1B^b H1E^b Cl2 5_666 0.96 2.84 3.70(3) 149.5 ?
C2B^b H2E^b Cl1 6_556 0.94(2) 2.98(3) 3.65(3) 129.6(17) ?
C2B^b H2E^b Cl1 4_455 0.94(2) 2.98(3) 3.65(3) 129.6(17) ?


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: H2O/HCl'
####################################################################### 
# 
# 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_19CGC005CT150K
_database_code_depnum_ccdc_archive 'CCDC 2000623'
loop_
_audit_author_name
_audit_author_address
'Antonio L. Llamas-Saiz'
;Universidade de Santiago de Compostela
Spain
;
_audit_update_record             
;
2020-05-02 deposited with the CCDC.	2020-08-29 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            '[TMS][FeCl4] - T150K'
_chemical_formula_moiety         'C3 H9 S, Cl4 Fe'
_chemical_formula_sum            'C3 H9 Cl4 Fe S'
_chemical_formula_iupac          ?
_chemical_formula_weight         274.81

_chemical_melting_point          ?

_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
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                   12.2667(8)
_cell_length_b                   7.9320(5)
_cell_length_c                   11.3580(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1105.13(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8200
_cell_measurement_theta_min      2.4438
_cell_measurement_theta_max      32.5214
_cell_measurement_temperature    150.(2)

_exptl_crystal_description       block
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.056
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             548

_exptl_absorpt_coefficient_mu    2.452
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_T_max  0.88

_exptl_special_details           
;
;

_diffrn_ambient_temperature      150.(2)

_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS 3.0'

_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'multilayer mirror'

_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON-III C14'
_diffrn_measurement_method       'φ or ω oscillation scans'

_diffrn_detector_area_resol_mean 7.3910

_diffrn_reflns_number            16182
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_theta_min         2.44
_diffrn_reflns_theta_max         33.16
_diffrn_reflns_theta_full        33.16
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17

_refine_special_details          
;
;

_reflns_number_total             2241
_reflns_number_gt                1726
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0345
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0680
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.040
_refine_ls_number_reflns         2241
_refine_ls_number_parameters     83
_refine_ls_number_restraints     94
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0142P)²+1.2123P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.469
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_computing_data_collection       'Bruker APEX3 software'
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'ORTEP 2014.1 (Farrugia, 2012)'
_computing_publication_material  'IUCr Journals printCIF'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe1 0.49776(3) 0.75 0.27481(3) 0.02546(9) Uani d T P S 1.0 . .
Cl Cl1 0.44375(4) 0.52089(7) 0.18353(5) 0.03959(13) Uani d . . . 1.0 . .
Cl Cl2 0.67738(5) 0.75 0.26954(6) 0.03096(14) Uani d T P S 1.0 . .
Cl Cl3 0.44632(7) 0.75 0.45892(7) 0.03955(17) Uani d T P S 1.0 . .
S S1^a 0.16553(6) 0.25 0.40126(7) 0.02749(18) Uani d TU P DS 0.923(2) A 1
C C1^a 0.2477(5) 0.4235(6) 0.4415(5) 0.0417(10) Uani d U P D 0.923(2) A 1
H H1A^a 0.320512 0.410131 0.407345 0.063 Uiso calc U P DR 0.923(2) A 1
H H1B^a 0.253423 0.428961 0.527468 0.063 Uiso calc U P DR 0.923(2) A 1
H H1C^a 0.214619 0.527788 0.412 0.063 Uiso calc U P DR 0.923(2) A 1
C C2^a 0.1821(6) 0.25 0.2427(4) 0.0368(12) Uani d TU P DS 0.923(2) A 1
H H2A^a 0.1462(17) 0.3504(12) 0.2141(18) 0.055 Uiso d U P D 0.923(2) A 1
H H2B^a 0.2587(15) 0.25 0.226(2) 0.055 Uiso d U P DS 0.923(2) A 1
S S1B^b 0.2888(9) 0.25 0.3646(8) 0.035(2) Uani d TU P DS 0.077(2) A 2
C C1B^b 0.257(4) 0.426(5) 0.452(5) 0.025(5) Uani d U P D 0.077(2) A 2
H H1D^b 0.281741 0.529342 0.41251 0.038 Uiso calc U P R 0.077(2) A 2
H H1E^b 0.294426 0.416472 0.528491 0.038 Uiso calc U P R 0.077(2) A 2
H H1F^b 0.178391 0.431798 0.464983 0.038 Uiso calc U P R 0.077(2) A 2
C C2B^b 0.178(5) 0.25 0.261(6) 0.028(6) Uani d TU P DS 0.077(2) A 2
H H2D^b 0.185(8) 0.3506(12) 0.213(6) 0.041 Uiso d U P D 0.077(2) A 2
H H2E^b 0.111(3) 0.25 0.305(10) 0.041 Uiso d U P DS 0.077(2) A 2


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 Cl3 . 2.1843(8) ?
Fe1 Cl1 . 2.1946(6) ?
Fe1 Cl1_$1 7_575 2.1946(6) ?
Fe1 Cl2 . 2.2042(7) ?
S1^a C1^a_$2 7_565 1.766(4) ?
S1^a C1^a . 1.766(4) ?
S1^a C2^a . 1.812(5) ?
C1^a H1A^a . 0.98 ?
C1^a H1B^a . 0.98 ?
C1^a H1C^a . 0.98 ?
C2^a H2A^a . 0.966(12) ?
C2^a H2B^a . 0.958(16) ?
C2^a H2A^a_$2 7_565 0.966(11) ?
C2^a H2D^b_$2 7_565 0.87(3) ?
S1B^b C1B^b . 1.761(19) ?
S1B^b C1B^b_$2 7_565 1.761(19) ?
S1B^b C2B^b . 1.804(19) ?
C1B^b H1D^b . 0.98 ?
C1B^b H1E^b . 0.98 ?
C1B^b H1F^b . 0.98 ?
C2B^b H2D^b . 0.970(14) ?
C2B^b H2E^b . 0.965(19) ?
C2B^b H2D^b_$2 7_565 0.970(14) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl3 Fe1 Cl1 . . 111.41(2) ?
Cl3 Fe1 Cl1_$1 . 7_575 111.41(2) ?
Cl1 Fe1 Cl1_$1 . 7_575 111.80(4) ?
Cl3 Fe1 Cl2 . . 108.34(3) ?
Cl1 Fe1 Cl2 . . 106.80(2) ?
Cl1 Fe1 Cl2 7_575 . 106.80(2) ?
C1^a S1^a C1^a 7_565 . 102.4(3) ?
C1^a S1^a C2^a 7_565 . 101.1(3) ?
C1^a S1^a C2^a . . 101.1(3) ?
S1^a C1^a H1A^a . . 109.5 ?
S1^a C1^a H1B^a . . 109.5 ?
H1A^a C1^a H1B^a . . 109.5 ?
S1^a C1^a H1C^a . . 109.5 ?
H1A^a C1^a H1C^a . . 109.5 ?
H1B^a C1^a H1C^a . . 109.5 ?
S1^a C2^a H2A^a . . 106.5(13) ?
S1^a C2^a H2B^a . . 107.7(17) ?
H2A^a C2^a H2B^a . . 112.4(15) ?
S1^a C2^a H2A^a_$2 . 7_565 106.5(13) ?
H2A^a C2^a H2A^a_$2 . 7_565 111.(2) ?
H2B^a C2^a H2A^a_$2 . 7_565 112.4(15) ?
S1^a C2^a H2D^b_$2 . 7_565 113.(5) ?
H2A^a C2^a H2D^b_$2 . 7_565 130.(3) ?
H2B^a C2^a H2D^b_$2 . 7_565 83.(7) ?
C1B^b S1B^b C1B^b_$2 . 7_565 105.(4) ?
C1B^b S1B^b C2B^b . . 101.8(14) ?
C1B^b S1B^b C2B^b 7_565 . 101.8(14) ?
S1B^b C1B^b H1D^b . . 109.5 ?
S1B^b C1B^b H1E^b . . 109.5 ?
H1D^b C1B^b H1E^b . . 109.5 ?
S1B^b C1B^b H1F^b . . 109.5 ?
H1D^b C1B^b H1F^b . . 109.5 ?
H1E^b C1B^b H1F^b . . 109.5 ?
S1B^b C2B^b H2D^b . . 107.2(19) ?
S1B^b C2B^b H2E^b . . 108.(2) ?
H2D^b C2B^b H2E^b . . 112.(2) ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C1^a H1B^a Cl2 5_666 0.98 2.84 3.676(6) 144.0 ?
C1^a H1C^a Cl2 6_556 0.98 2.75 3.632(6) 150.0 ?
C1B^b H1D^b Cl2 6_556 0.98 3.0 3.73(6) 132.4 ?
C1B^b H1D^b Cl3 . 0.98 2.72 3.46(5) 132.2 ?
C1B^b H1E^b Cl2 5_666 0.98 2.67 3.55(6) 149.1 ?
C1B^b H1F^b Cl1 2_565 0.98 2.92 3.63(5) 129.5 ?
C2B^b H2E^b Cl1 6_556 0.965(19) 2.97(3) 3.64(6) 128.(3) ?
C2B^b H2E^b Cl1 4_455 0.965(19) 2.97(3) 3.64(6) 128.(3) ?


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: H2O/HCl'
####################################################################### 
# 
# 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_19CGC005CT200K
_database_code_depnum_ccdc_archive 'CCDC 2000619'
loop_
_audit_author_name
_audit_author_address
'Antonio L. Llamas-Saiz'
;Universidade de Santiago de Compostela
Spain
;
_audit_update_record             
;
2020-05-02 deposited with the CCDC.	2020-08-29 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            '[TMS][FeCl4] - T200K'
_chemical_formula_moiety         'C3 H9 S, Cl4 Fe'
_chemical_formula_sum            'C3 H9 Cl4 Fe S'
_chemical_formula_iupac          ?
_chemical_formula_weight         274.81

_chemical_melting_point          ?

_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
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                   12.4012(4)
_cell_length_b                   7.9136(2)
_cell_length_c                   11.4326(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1121.97(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7037
_cell_measurement_theta_min      2.4230
_cell_measurement_theta_max      31.2763
_cell_measurement_temperature    200.(2)

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.171
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.056
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             548

_exptl_absorpt_coefficient_mu    2.415
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_T_max  0.88

_exptl_special_details           
;
;

_diffrn_ambient_temperature      200.(2)

_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS 3.0'

_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'multilayer mirror'

_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON-III C14'
_diffrn_measurement_method       'φ or ω oscillation scans'

_diffrn_detector_area_resol_mean 7.3910

_diffrn_reflns_number            17487
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_theta_min         2.42
_diffrn_reflns_theta_max         33.13
_diffrn_reflns_theta_full        33.13
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17

_refine_special_details          
;
;

_reflns_number_total             2260
_reflns_number_gt                1715
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0343
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0827
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.025
_refine_ls_number_reflns         2260
_refine_ls_number_parameters     83
_refine_ls_number_restraints     94
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0265P)²+0.7030P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.410
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_computing_data_collection       'Bruker APEX3 software'
_computing_cell_refinement       'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'ORTEP 2014.1 (Farrugia, 2012)'
_computing_publication_material  'IUCr Journals printCIF'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe1 0.49766(3) 0.75 0.27699(3) 0.03978(11) Uani d T P S 1.0 . .
Cl Cl1 0.44404(5) 0.52137(8) 0.18601(6) 0.06360(17) Uani d . . . 1.0 . .
Cl Cl2 0.67519(5) 0.75 0.27311(6) 0.04901(17) Uani d T P S 1.0 . .
Cl Cl3 0.44527(8) 0.75 0.45892(7) 0.0656(2) Uani d T P S 1.0 . .
S S1^a 0.16446(7) 0.25 0.39896(7) 0.0424(2) Uani d TU P DS 0.811(2) A 1
C C1^a 0.2432(6) 0.4213(7) 0.4415(6) 0.0744(17) Uani d U P D 0.811(2) A 1
H H1A^a 0.316848 0.406277 0.412354 0.112 Uiso calc U P DR 0.811(2) A 1
H H1B^a 0.244301 0.428634 0.527081 0.112 Uiso calc U P DR 0.811(2) A 1
H H1C^a 0.21266 0.525506 0.409098 0.112 Uiso calc U P DR 0.811(2) A 1
C C2^a 0.1800(5) 0.25 0.2428(5) 0.0525(16) Uani d TU P DS 0.811(2) A 1
H H2A^a 0.1450(18) 0.3511(12) 0.220(2) 0.079 Uiso d U P D 0.811(2) A 1
H H2B^a 0.2563(15) 0.25 0.231(3) 0.079 Uiso d U P DS 0.811(2) A 1
S S1B^b 0.2845(4) 0.25 0.3650(3) 0.0552(12) Uani d TU P DS 0.189(2) A 2
C C1B^b 0.2441(18) 0.433(2) 0.4389(16) 0.044(4) Uani d U P D 0.189(2) A 2
H H1D^b 0.268586 0.532345 0.395625 0.067 Uiso calc U P R 0.189(2) A 2
H H1E^b 0.275833 0.433384 0.517445 0.067 Uiso calc U P R 0.189(2) A 2
H H1F^b 0.16532 0.434446 0.445172 0.067 Uiso calc U P R 0.189(2) A 2
C C2B^b 0.207(2) 0.25 0.2346(17) 0.047(5) Uani d TU P DS 0.189(2) A 2
H H2D^b 0.228(4) 0.3512(12) 0.195(2) 0.071 Uiso d U P D 0.189(2) A 2
H H2E^b 0.133(2) 0.25 0.261(4) 0.071 Uiso d U P DS 0.189(2) A 2


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 Cl3 . 2.1790(9) ?
Fe1 Cl1 . 2.1904(6) ?
Fe1 Cl1_$1 7_575 2.1904(6) ?
Fe1 Cl2 . 2.2020(8) ?
S1^a C1^a . 1.740(5) ?
S1^a C1^a_$2 7_565 1.740(5) ?
S1^a C2^a . 1.796(6) ?
C1^a H1A^a . 0.98 ?
C1^a H1B^a . 0.98 ?
C1^a H1C^a . 0.98 ?
C2^a H2A^a . 0.947(12) ?
C2^a H2B^a . 0.956(16) ?
C2^a H2A^a_$2 7_565 0.947(12) ?
C2^a H2D^b_$2 7_565 1.14(3) ?
S1B^b C1B^b . 1.747(15) ?
S1B^b C2B^b . 1.772(15) ?
C1B^b H1D^b . 0.98 ?
C1B^b H1E^b . 0.98 ?
C1B^b H1F^b . 0.98 ?
C2B^b H2D^b . 0.955(14) ?
C2B^b H2E^b . 0.963(18) ?
C2B^b H2D^b_$2 7_565 0.955(14) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl3 Fe1 Cl1 . . 111.27(2) ?
Cl3 Fe1 Cl1_$1 . 7_575 111.27(2) ?
Cl1 Fe1 Cl1_$1 . 7_575 111.39(4) ?
Cl3 Fe1 Cl2 . . 108.50(4) ?
Cl1 Fe1 Cl2 . . 107.09(2) ?
Cl1 Fe1 Cl2 7_575 . 107.09(2) ?
C1^a S1^a C1^a_$2 . 7_565 102.4(5) ?
C1^a S1^a C2^a . . 102.6(3) ?
C1^a S1^a C2^a 7_565 . 102.6(3) ?
S1^a C1^a H1A^a . . 109.5 ?
S1^a C1^a H1B^a . . 109.5 ?
H1A^a C1^a H1B^a . . 109.5 ?
S1^a C1^a H1C^a . . 109.5 ?
H1A^a C1^a H1C^a . . 109.5 ?
H1B^a C1^a H1C^a . . 109.5 ?
S1^a C2^a H2A^a . . 103.2(16) ?
S1^a C2^a H2B^a . . 104.(2) ?
H2A^a C2^a H2B^a . . 114.5(16) ?
S1^a C2^a H2A^a_$2 . 7_565 103.2(16) ?
H2A^a C2^a H2A^a_$2 . 7_565 115.(2) ?
H2B^a C2^a H2A^a_$2 . 7_565 114.5(16) ?
S1^a C2^a H2D^b_$2 . 7_565 122.4(14) ?
H2A^a C2^a H2D^b_$2 . 7_565 134.(3) ?
H2B^a C2^a H2D^b_$2 . 7_565 54.(2) ?
H2A^a C2^a H2D^b_$2 7_565 7_565 61.(3) ?
C1B^b S1B^b C2B^b . . 104.6(9) ?
S1B^b C1B^b H1D^b . . 109.5 ?
S1B^b C1B^b H1E^b . . 109.5 ?
H1D^b C1B^b H1E^b . . 109.5 ?
S1B^b C1B^b H1F^b . . 109.5 ?
H1D^b C1B^b H1F^b . . 109.5 ?
H1E^b C1B^b H1F^b . . 109.5 ?
S1B^b C2B^b H2D^b . . 105.(2) ?
S1B^b C2B^b H2E^b . . 105.(2) ?
H2D^b C2B^b H2E^b . . 114.(2) ?
H2A^a C2B^b H2D^b_$2 7_565 7_565 61.(3) ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C1^a H1B^a Cl2 5_666 0.98 2.87 3.675(7) 140.5 ?
C1^a H1C^a Cl2 6_556 0.98 2.78 3.674(7) 152.5 ?
C1B^b H1D^b Cl2 6_556 0.98 2.83 3.59(2) 135.0 ?
C1B^b H1D^b Cl3 . 0.98 2.88 3.547(16) 126.2 ?
C1B^b H1E^b Cl2 5_666 0.98 2.87 3.73(2) 147.9 ?


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: H2O/HCl'
####################################################################### 
# 
# 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_19CGC005CT100K
_database_code_depnum_ccdc_archive 'CCDC 2000620'
loop_
_audit_author_name
_audit_author_address
'Antonio L. Llamas-Saiz'
;Universidade de Santiago de Compostela
Spain
;
_audit_update_record             
;
2020-05-02 deposited with the CCDC.	2020-08-29 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            '[TMS][FeCl4] - T100K'
_chemical_formula_moiety         'Cl4 Fe, C3 H9 S'
_chemical_formula_sum            'C3 H9 Cl4 Fe S'
_chemical_formula_iupac          ?
_chemical_formula_weight         274.81

_chemical_melting_point          ?

_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x+1/2, -y, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'
'x-1/2, y, -z-1/2'

_cell_length_a                   12.1950(7)
_cell_length_b                   7.9217(4)
_cell_length_c                   11.3013(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1091.76(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9890
_cell_measurement_theta_min      3.1404
_cell_measurement_theta_max      36.2105
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       block
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.056
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             548

_exptl_absorpt_coefficient_mu    2.482
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_T_max  0.87

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS 3.0'

_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'multilayer mirror'

_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON-III C14'
_diffrn_measurement_method       'φ or ω oscillation scans'

_diffrn_detector_area_resol_mean 7.3910

_diffrn_reflns_number            65618
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0154
_diffrn_reflns_theta_min         2.46
_diffrn_reflns_theta_max         36.37
_diffrn_reflns_theta_full        36.37
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18

_refine_special_details          
;
;

_reflns_number_total             2802
_reflns_number_gt                2420
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0288
_refine_ls_wR_factor_gt          0.0603
_refine_ls_wR_factor_ref         0.0652
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_restrained_S_all      1.102
_refine_ls_number_reflns         2802
_refine_ls_number_parameters     63
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0238P)²+0.7796P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.657
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_computing_data_collection       'Bruker APEX3 software'
_computing_cell_refinement       'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'ORTEP 2014.1 (Farrugia, 2012)'
_computing_publication_material  'IUCr Journals printCIF'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe1 0.49726(2) 0.75 0.27343(2) 0.01650(5) Uani d T P S 1 . .
Cl Cl1 0.44320(3) 0.51987(4) 0.18187(3) 0.02465(7) Uani d . . . 1 . .
Cl Cl2 0.67804(3) 0.75 0.26756(4) 0.01992(8) Uani d T P S 1 . .
Cl Cl3 0.44645(4) 0.75 0.45920(4) 0.02468(9) Uani d T P S 1 . .
S S1 0.16629(4) 0.25 0.40316(4) 0.01866(8) Uani d T P S 1 . .
C C1 0.25123(13) 0.42435(18) 0.44350(13) 0.0257(3) Uani d . . . 1 . .
H H1A 0.3228(17) 0.410(3) 0.4059(19) 0.039 Uiso d U . . 1 . .
H H1B 0.2553(15) 0.423(3) 0.5294(19) 0.039 Uiso d U . . 1 . .
H H1C 0.2182(17) 0.521(3) 0.4151(19) 0.039 Uiso d U . . 1 . .
C C2 0.18047(18) 0.25 0.24533(17) 0.0239(3) Uani d T P S 1 . .
H H2A 0.1448(17) 0.347(3) 0.2155(17) 0.036 Uiso d U . . 1 . .
H H2B 0.254(2) 0.25 0.226(3) 0.036 Uiso d U P S 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 Cl3 . 2.1890(5) ?
Fe1 Cl1 7_575 2.1974(4) ?
Fe1 Cl1 . 2.1974(4) ?
Fe1 Cl2 . 2.2056(5) ?
S1 C1 . 1.7856(14) ?
S1 C1 7_565 1.7856(14) ?
S1 C2 . 1.792(2) ?
C1 H1A . 0.98(2) ?
C1 H1B . 0.97(2) ?
C1 H1C . 0.92(2) ?
C2 H2A . 0.94(2) ?
C2 H2B . 0.92(3) ?
C2 H2A 7_565 0.94(2) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl3 Fe1 Cl1 . 7_575 111.513(13) ?
Cl3 Fe1 Cl1 . . 111.513(13) ?
Cl1 Fe1 Cl1 7_575 . 112.11(2) ?
Cl3 Fe1 Cl2 . . 108.17(2) ?
Cl1 Fe1 Cl2 7_575 . 106.603(12) ?
Cl1 Fe1 Cl2 . . 106.604(12) ?
C1 S1 C1 . 7_565 101.34(10) ?
C1 S1 C2 . . 101.43(7) ?
C1 S1 C2 7_565 . 101.43(7) ?
S1 C1 H1A . . 108.5(13) ?
S1 C1 H1B . . 106.2(13) ?
H1A C1 H1B . . 112.8(17) ?
S1 C1 H1C . . 107.4(14) ?
H1A C1 H1C . . 109.6(18) ?
H1B C1 H1C . . 112.2(19) ?
S1 C2 H2A . . 108.1(12) ?
S1 C2 H2B . . 109.1(19) ?
H2A C2 H2B . . 111.4(16) ?
S1 C2 H2A . 7_565 108.1(12) ?
H2A C2 H2A . 7_565 109.(3) ?
H2B C2 H2A . 7_565 111.4(16) ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C1 H1B Cl2 5_666 0.97(2) 2.79(2) 3.6488(15) 147.0(17) ?
C1 H1C Cl2 2_465 0.92(2) 2.79(2) 3.6251(15) 150.9(17) ?


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: H2O/HCl'
####################################################################### 
# 
# 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_19CGC005CT310K
_database_code_depnum_ccdc_archive 'CCDC 2000621'
loop_
_audit_author_name
_audit_author_address
'Antonio L. Llamas-Saiz'
;Universidade de Santiago de Compostela
Spain
;
_audit_update_record             
;
2020-05-02 deposited with the CCDC.	2020-08-29 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            '[TMS][FeCl4] - T310K'
_chemical_formula_moiety         'C3 H9 S, Cl4 Fe'
_chemical_formula_sum            'C3 H9 Cl4 Fe S'
_chemical_formula_iupac          ?
_chemical_formula_weight         274.81

_chemical_melting_point          ?

_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
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                   12.7698(9)
_cell_length_b                   7.9044(5)
_cell_length_c                   11.5756(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1168.41(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3854
_cell_measurement_theta_min      2.3748
_cell_measurement_theta_max      22.5571
_cell_measurement_temperature    310.(2)

_exptl_crystal_description       block
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_size_max          0.171
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.056
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             548

_exptl_absorpt_coefficient_mu    2.319
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_T_max  0.88

_exptl_special_details           
;
;

_diffrn_ambient_temperature      310.(2)

_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS 3.0'

_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'multilayer mirror'

_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON-III C14'
_diffrn_measurement_method       'φ or ω oscillation scans'

_diffrn_detector_area_resol_mean 7.3910

_diffrn_reflns_number            11256
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_theta_min         2.38
_diffrn_reflns_theta_max         26.72
_diffrn_reflns_theta_full        26.72
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14

_refine_special_details          
;
;

_reflns_number_total             1324
_reflns_number_gt                844
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0378
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.1113
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      0.995
_refine_ls_number_reflns         1324
_refine_ls_number_parameters     121
_refine_ls_number_restraints     219
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0403P)²+0.7773P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.230
_refine_diff_density_min         -0.215
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_computing_data_collection       'Bruker APEX3 software'
_computing_cell_refinement       'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'ORTEP 2014.1 (Farrugia, 2012)'
_computing_publication_material  'IUCr Journals printCIF'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe1 0.49614(6) 0.75 0.27996(7) 0.0843(3) Uani d T P S 1.0 . .
Cl Cl1 0.44408(10) 0.52362(18) 0.18902(13) 0.1339(5) Uani d . . . 1.0 . .
Cl Cl2 0.66780(11) 0.75 0.27993(15) 0.1096(5) Uani d T P S 1.0 . .
Cl Cl3 0.43972(19) 0.75 0.45625(16) 0.1462(8) Uani d T P S 1.0 . .
S S1^a 0.1644(2) 0.25 0.3946(2) 0.0881(8) Uani d TU P DS 0.600(3) A 1
C C1^a 0.2214(8) 0.4226(14) 0.4416(10) 0.113(3) Uani d U P D 0.600(3) A 1
H H1A^a 0.294145 0.420643 0.420704 0.169 Uiso calc U P DR 0.600(3) A 1
H H1B^a 0.21504 0.428483 0.524131 0.169 Uiso calc U P DR 0.600(3) A 1
H H1C^a 0.188428 0.519588 0.407473 0.169 Uiso calc U P DR 0.600(3) A 1
C C2^a 0.2026(11) 0.25 0.2345(8) 0.095(4) Uani d TU P DS 0.600(3) A 1
H H2A^a 0.175(3) 0.3498(13) 0.203(3) 0.142 Uiso d U P D 0.600(3) A 1
H H2B^a 0.2771(19) 0.25 0.231(3) 0.142 Uiso d U P DS 0.600(3) A 1
S S1B^b 0.2797(6) 0.25 0.3669(6) 0.0877(17) Uani d TU P DS 0.257(3) B 2
C C1B^b 0.2626(16) 0.425(3) 0.435(2) 0.095(4) Uani d U P D 0.257(3) B 2
H H1D^b 0.298813 0.514001 0.394873 0.143 Uiso calc U P R 0.257(3) B 2
H H1E^b 0.289575 0.414707 0.511663 0.143 Uiso calc U P R 0.257(3) B 2
H H1F^b 0.189173 0.450484 0.437659 0.143 Uiso calc U P R 0.257(3) B 2
C C2B^b 0.172(3) 0.25 0.252(2) 0.090(5) Uani d TU P DS 0.257(3) B 2
H H2D^b 0.180(4) 0.3496(13) 0.208(3) 0.135 Uiso d U P D 0.257(3) B 2
H H2E^b 0.107(2) 0.25 0.292(5) 0.135 Uiso d U P DS 0.257(3) B 2
S S1C^c 0.2339(16) 0.319(3) 0.3630(17) 0.097(3) Uani d U P D 0.0711(14) C -3
C C1C^c 0.144(3) 0.356(8) 0.459(3) 0.094(5) Uani d U P D 0.0711(14) C -3
H H1G^c 0.175995 0.384712 0.53165 0.141 Uiso calc U P R 0.0711(14) C -3
H H1H^c 0.101046 0.257108 0.469101 0.141 Uiso calc U P R 0.0711(14) C -3
H H1I^c 0.10056 0.448719 0.434154 0.141 Uiso calc U P R 0.0711(14) C -3
C C2C^c 0.156(4) 0.276(10) 0.228(3) 0.089(6) Uani d U P D 0.0711(14) C -3
H H1J^c 0.114243 0.176063 0.238485 0.134 Uiso calc U P DR 0.0711(14) C -3
H H1K^c 0.203058 0.258742 0.16396 0.134 Uiso calc U P R 0.0711(14) C -3
H H1L^c 0.111222 0.370374 0.211567 0.134 Uiso calc U P R 0.0711(14) C -3
C C3C^c 0.335(3) 0.198(6) 0.384(5) 0.095(7) Uani d U P D 0.0711(14) C -3
H H1M^c 0.392251 0.23615 0.337175 0.143 Uiso calc U P R 0.0711(14) C -3
H H1N^c 0.317581 0.083583 0.363672 0.143 Uiso calc U P R 0.0711(14) C -3
H H1O^c 0.354858 0.202273 0.464078 0.143 Uiso calc U P R 0.0711(14) C -3


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 Cl3 . 2.1641(19) ?
Fe1 Cl1_$1 7_575 2.1799(13) ?
Fe1 Cl1 . 2.1799(13) ?
Fe1 Cl2 . 2.1921(17) ?
S1^a C1^a . 1.639(8) ?
S1^a C1^a_$2 7_565 1.639(8) ?
S1^a C2^a . 1.917(11) ?
C1^a H1A^a . 0.96 ?
C1^a H1B^a . 0.96 ?
C1^a H1C^a . 0.96 ?
C2^a H2A^a . 0.938(15) ?
C2^a H2B^a . 0.952(19) ?
C2^a H2A^a_$2 7_565 0.938(15) ?
S1B^b C1B^b_$2 7_565 1.603(14) ?
S1B^b C1B^b . 1.603(14) ?
S1B^b C2B^b . 1.908(17) ?
C1B^b H1D^b . 0.96 ?
C1B^b H1E^b . 0.96 ?
C1B^b H1F^b . 0.96 ?
C2B^b H2D^b . 0.944(15) ?
C2B^b H2E^b . 0.95(2) ?
S1C^c C3C^c . 1.627(18) ?
S1C^c C1C^c . 1.631(18) ?
S1C^c C2C^c . 1.887(17) ?
C1C^c H1G^c . 0.96 ?
C1C^c H1H^c . 0.96 ?
C1C^c H1I^c . 0.96 ?
C2C^c H1J^c . 0.96 ?
C2C^c H1K^c . 0.96 ?
C2C^c H1L^c . 0.96 ?
C3C^c H1M^c . 0.96 ?
C3C^c H1N^c . 0.96 ?
C3C^c H1O^c . 0.96 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl3 Fe1 Cl1_$1 . 7_575 110.72(6) ?
Cl3 Fe1 Cl1 . . 110.72(6) ?
Cl1 Fe1 Cl1 7_575 . 110.34(9) ?
Cl3 Fe1 Cl2 . . 109.46(9) ?
Cl1 Fe1 Cl2 7_575 . 107.75(5) ?
Cl1 Fe1 Cl2 . . 107.75(5) ?
C1^a S1^a C1^a_$2 . 7_565 112.6(9) ?
C1^a S1^a C2^a . . 102.0(5) ?
C1^a S1^a C2^a 7_565 . 102.0(5) ?
S1^a C1^a H1A^a . . 109.5 ?
S1^a C1^a H1B^a . . 109.5 ?
H1A^a C1^a H1B^a . . 109.5 ?
S1^a C1^a H1C^a . . 109.5 ?
H1A^a C1^a H1C^a . . 109.5 ?
H1B^a C1^a H1C^a . . 109.5 ?
S1^a C2^a H2A^a . . 106.(2) ?
S1^a C2^a H2B^a . . 107.(2) ?
H2A^a C2^a H2B^a . . 111.(2) ?
S1^a C2^a H2A^a_$2 . 7_565 106.(2) ?
H2A^a C2^a H2A^a_$2 . 7_565 114.(3) ?
H2B^a C2^a H2A^a_$2 . 7_565 111.(2) ?
C1B^b S1B^b C1B^b 7_565 . 119.(2) ?
C1B^b S1B^b C2B^b 7_565 . 104.0(9) ?
C1B^b S1B^b C2B^b . . 104.0(9) ?
S1B^b C1B^b H1D^b . . 109.5 ?
S1B^b C1B^b H1E^b . . 109.5 ?
H1D^b C1B^b H1E^b . . 109.5 ?
S1B^b C1B^b H1F^b . . 109.5 ?
H1D^b C1B^b H1F^b . . 109.5 ?
H1E^b C1B^b H1F^b . . 109.5 ?
S1B^b C2B^b H2D^b . . 107.(2) ?
S1B^b C2B^b H2E^b . . 107.(2) ?
H2D^b C2B^b H2E^b . . 111.(2) ?
C3C^c S1C^c C1C^c . . 124.(3) ?
C3C^c S1C^c C2C^c . . 116.(3) ?
C1C^c S1C^c C2C^c . . 103.2(13) ?
S1C^c C1C^c H1G^c . . 109.5 ?
S1C^c C1C^c H1H^c . . 109.5 ?
H1G^c C1C^c H1H^c . . 109.5 ?
S1C^c C1C^c H1I^c . . 109.5 ?
H1G^c C1C^c H1I^c . . 109.5 ?
H1H^c C1C^c H1I^c . . 109.5 ?
S1C^c C2C^c H1J^c . . 109.5 ?
S1C^c C2C^c H1K^c . . 109.5 ?
H1J^c C2C^c H1K^c . . 109.5 ?
S1C^c C2C^c H1L^c . . 109.5 ?
H1J^c C2C^c H1L^c . . 109.5 ?
H1K^c C2C^c H1L^c . . 109.5 ?
S1C^c C3C^c H1M^c . . 109.5 ?
S1C^c C3C^c H1N^c . . 109.5 ?
H1M^c C3C^c H1N^c . . 109.5 ?
S1C^c C3C^c H1O^c . . 109.5 ?
H1M^c C3C^c H1O^c . . 109.5 ?
H1N^c C3C^c H1O^c . . 109.5 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C1^a H1B^a Cl1 2_565 0.96 2.81 3.585(11) 138.0 ?
C1^a H1C^a Cl2 6_556 0.96 2.84 3.707(14) 150.0 ?
C1B^b H1D^b Cl3 . 0.96 2.69 3.43(2) 134.9 ?
C1B^b H1E^b Cl2 5_666 0.96 2.79 3.69(3) 155.7 ?
C1C^c H1G^c Cl1 2_565 0.96 2.49 3.04(3) 116.1 ?
C1C^c H1I^c Cl1 6_556 0.96 2.53 3.35(5) 143.4 ?
C2C^c H1J^c Cl1 4_455 0.96 2.81 3.72(6) 158.3 ?
C2C^c H1L^c Cl1 6_556 0.96 2.71 3.48(7) 137.3 ?
C3C^c H1M^c Cl1 . 0.96 2.92 3.70(6) 138.6 ?
C3C^c H1O^c Cl3 5_666 0.96 2.81 3.44(4) 124.6 ?


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: H2O/HCl'
####################################################################### 
# 
# 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_19CGC005CT250K
_database_code_depnum_ccdc_archive 'CCDC 2000622'
loop_
_audit_author_name
_audit_author_address
'Antonio L. Llamas-Saiz'
;Universidade de Santiago de Compostela
Spain
;
_audit_update_record             
;
2020-05-02 deposited with the CCDC.	2020-08-29 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            '[TMS][FeCl4] - T250K'
_chemical_formula_moiety         'C3 H9 S, Cl4 Fe'
_chemical_formula_sum            'C3 H9 Cl4 Fe S'
_chemical_formula_iupac          ?
_chemical_formula_weight         274.81

_chemical_melting_point          ?

_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
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                   12.5644(5)
_cell_length_b                   7.8927(3)
_cell_length_c                   11.5059(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1141.01(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5252
_cell_measurement_theta_min      2.4002
_cell_measurement_theta_max      26.6786
_cell_measurement_temperature    250.(2)

_exptl_crystal_description       block
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_size_max          0.171
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.056
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             548

_exptl_absorpt_coefficient_mu    2.375
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_T_max  0.88

_exptl_special_details           
;
;

_diffrn_ambient_temperature      250.(2)

_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS 3.0'

_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'multilayer mirror'

_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON-III C14'
_diffrn_measurement_method       'φ or ω oscillation scans'

_diffrn_detector_area_resol_mean 7.3910

_diffrn_reflns_number            13914
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_theta_min         2.40
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_full        29.57
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15

_refine_special_details          
;
;

_reflns_number_total             1702
_reflns_number_gt                1194
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0401
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.1090
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.018
_refine_ls_number_reflns         1702
_refine_ls_number_parameters     83
_refine_ls_number_restraints     94
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0406P)²+0.9045P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.374
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_computing_data_collection       'Bruker APEX3 software'
_computing_cell_refinement       'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'ORTEP 2014.1 (Farrugia, 2012)'
_computing_publication_material  'IUCr Journals printCIF'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe1 0.49706(4) 0.75 0.27889(5) 0.0574(2) Uani d T P S 1.0 . .
Cl Cl1 0.44397(7) 0.52192(13) 0.18813(10) 0.0929(3) Uani d . . . 1.0 . .
Cl Cl2 0.67193(8) 0.75 0.27691(11) 0.0726(3) Uani d T P S 1.0 . .
Cl Cl3 0.44308(14) 0.75 0.45806(11) 0.0997(5) Uani d T P S 1.0 . .
S S1^a 0.16402(12) 0.25 0.39668(13) 0.0627(5) Uani d TU P DS 0.714(3) A 1
C C1^a 0.2334(13) 0.4204(13) 0.4422(11) 0.103(4) Uani d U P D 0.714(3) A 1
H H1A^a 0.307387 0.408219 0.419707 0.155 Uiso calc U P DR 0.714(3) A 1
H H1B^a 0.228509 0.429136 0.526138 0.155 Uiso calc U P DR 0.714(3) A 1
H H1C^a 0.204153 0.521915 0.406996 0.155 Uiso calc U P DR 0.714(3) A 1
C C2^a 0.1794(9) 0.25 0.2420(7) 0.071(3) Uani d TU P DS 0.714(3) A 1
H H2A^a 0.145(2) 0.3504(12) 0.213(3) 0.106 Uiso d U P D 0.714(3) A 1
H H2B^a 0.2541(18) 0.25 0.225(3) 0.106 Uiso d U P DS 0.714(3) A 1
S S1B^b 0.2807(4) 0.25 0.3660(4) 0.0807(15) Uani d TU P DS 0.286(3) A 2
C C1B^b 0.250(3) 0.432(3) 0.434(2) 0.081(4) Uani d U P D 0.286(3) A 2
H H1D^b 0.269048 0.52685 0.384527 0.122 Uiso calc U P R 0.286(3) A 2
H H1E^b 0.290065 0.439059 0.506179 0.122 Uiso calc U P R 0.286(3) A 2
H H1F^b 0.174785 0.434647 0.450533 0.122 Uiso calc U P R 0.286(3) A 2
C C2B^b 0.207(3) 0.25 0.2337(16) 0.069(5) Uani d TU P DS 0.286(3) A 2
H H2D^b 0.226(4) 0.3505(13) 0.191(3) 0.103 Uiso d U P D 0.286(3) A 2
H H2E^b 0.132(3) 0.25 0.253(4) 0.103 Uiso d U P DS 0.286(3) A 2


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 Cl3 . 2.1703(14) ?
Fe1 Cl1_$1 7_575 2.1855(10) ?
Fe1 Cl1 . 2.1855(10) ?
Fe1 Cl2 . 2.1972(12) ?
S1^a C1^a_$2 7_565 1.686(10) ?
S1^a C1^a . 1.686(10) ?
S1^a C2^a . 1.790(9) ?
C1^a H1A^a . 0.97 ?
C1^a H1B^a . 0.97 ?
C1^a H1C^a . 0.97 ?
C2^a H2A^a . 0.964(15) ?
C2^a H2B^a . 0.958(18) ?
C2^a H2A^a_$2 7_565 0.964(15) ?
C2^a H2D^b_$2 7_565 1.15(4) ?
S1B^b C1B^b . 1.678(17) ?
S1B^b C1B^b_$2 7_565 1.678(17) ?
S1B^b C2B^b . 1.781(15) ?
C1B^b H1D^b . 0.97 ?
C1B^b H1E^b . 0.97 ?
C1B^b H1F^b . 0.97 ?
C2B^b H2D^b . 0.965(16) ?
C2B^b H2E^b . 0.962(19) ?
C2B^b H2D^b_$2 7_565 0.965(16) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl3 Fe1 Cl1_$1 . 7_575 111.01(4) ?
Cl3 Fe1 Cl1 . . 111.01(4) ?
Cl1 Fe1 Cl1 7_575 . 110.92(7) ?
Cl3 Fe1 Cl2 . . 108.81(6) ?
Cl1 Fe1 Cl2 7_575 . 107.47(3) ?
Cl1 Fe1 Cl2 . . 107.47(3) ?
C1^a S1^a C1^a 7_565 . 105.8(10) ?
C1^a S1^a C2^a 7_565 . 104.7(5) ?
C1^a S1^a C2^a . . 104.7(5) ?
S1^a C1^a H1A^a . . 109.5 ?
S1^a C1^a H1B^a . . 109.5 ?
H1A^a C1^a H1B^a . . 109.5 ?
S1^a C1^a H1C^a . . 109.5 ?
H1A^a C1^a H1C^a . . 109.5 ?
H1B^a C1^a H1C^a . . 109.5 ?
S1^a C2^a H2A^a . . 107.0(19) ?
S1^a C2^a H2B^a . . 108.(2) ?
H2A^a C2^a H2B^a . . 112.(2) ?
S1^a C2^a H2A^a_$2 . 7_565 107.0(19) ?
H2A^a C2^a H2A^a_$2 . 7_565 111.(3) ?
H2B^a C2^a H2A^a_$2 . 7_565 112.(2) ?
S1^a C2^a H2D^b_$2 . 7_565 124.3(16) ?
H2A^a C2^a H2D^b_$2 . 7_565 129.(3) ?
H2B^a C2^a H2D^b_$2 . 7_565 53.(2) ?
H2A^a C2^a H2D^b_$2 7_565 7_565 59.(3) ?
C1B^b S1B^b C1B^b_$2 . 7_565 118.(2) ?
C1B^b S1B^b C2B^b . . 106.3(10) ?
C1B^b S1B^b C2B^b 7_565 . 106.3(10) ?
S1B^b C1B^b H1D^b . . 109.5 ?
S1B^b C1B^b H1E^b . . 109.5 ?
H1D^b C1B^b H1E^b . . 109.5 ?
S1B^b C1B^b H1F^b . . 109.5 ?
H1D^b C1B^b H1F^b . . 109.5 ?
H1E^b C1B^b H1F^b . . 109.5 ?
S1B^b C2B^b H2D^b . . 108.(2) ?
S1B^b C2B^b H2E^b . . 108.(3) ?
H2D^b C2B^b H2E^b . . 111.(2) ?
H2A^a C2B^b H2D^b_$2 7_565 7_565 60.(3) ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C1^a H1B^a Cl1 2_565 0.97 2.88 3.630(15) 134.4 ?
C1^a H1B^a Cl2 5_666 0.97 2.95 3.697(14) 134.8 ?
C1^a H1C^a Cl2 6_556 0.97 2.81 3.704(14) 154.0 ?
C1B^b H1D^b Cl2 6_556 0.97 2.84 3.63(3) 139.5 ?
C1B^b H1D^b Cl3 . 0.97 2.93 3.50(3) 118.3 ?
C1B^b H1E^b Cl2 5_666 0.97 2.95 3.75(3) 141.1 ?


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: H2O/HCl'
