# Supplementary Information (SI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 2173682'
loop_
_audit_author_name
_audit_author_address
'Christoph Jessen'
;Ludwig Maximilian University Munich
Germany
;
_audit_update_record             
;
2022-05-19 deposited with the CCDC.	2024-09-10 downloaded from the CCDC.
;
_audit_block_code                ?
_audit_creation_method           SHELXL-2018/1
_audit_creation_date             2019-10-23
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'As F6, C2 H4 F O3'
_chemical_formula_sum            'C2 H4 As F7 O3'
_chemical_formula_weight         283.97

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   7.4858(3)
_cell_length_b                   8.0027(3)
_cell_length_c                   12.7743(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     765.27(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    121(2)
_cell_measurement_reflns_used    2404
_cell_measurement_theta_min      2.9920
_cell_measurement_theta_max      31.5680

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.465
_exptl_crystal_F_000             544
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    4.549
_shelx_estimated_absorpt_T_min   0.495
_shelx_estimated_absorpt_T_max   0.549
_exptl_absorpt_correction_T_min  0.80379
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;

_diffrn_ambient_temperature      121(2) # in K
_diffrn_source_type              'Spellman generator'
_diffrn_source_power             ? # in kW
_diffrn_source_voltage           50 # kV
_diffrn_source_current           40 # mA
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_collimation    0.5
_diffrn_measurement_device       'CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9809

_diffrn_reflns_number            8259
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.004
_diffrn_reflns_theta_max         32.238
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2544
_reflns_number_gt                2257
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.686
_reflns_Friedel_fraction_max     0.907
_reflns_Friedel_fraction_full    1.000

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0248P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.497(16)
_chemical_absolute_configuration RS
_refine_ls_number_reflns         2544
_refine_ls_number_parameters     135
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0320
_refine_ls_wR_factor_ref         0.0631
_refine_ls_wR_factor_gt          0.0587
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.027
_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
As1 As 0.69693(5) 0.45388(5) 0.19175(3) 0.01405(9) Uani 1 1 d . . . . .
F3 F 0.5630(3) 0.6078(3) 0.1386(2) 0.0256(6) Uani 1 1 d . . . . .
F4 F 0.5753(3) 0.4579(3) 0.30439(18) 0.0250(5) Uani 1 1 d . . . . .
F7 F 0.8276(3) 0.4582(3) 0.08139(16) 0.0223(5) Uani 1 1 d . . . . .
F1 F 0.6530(4) 0.9920(3) 0.5570(2) 0.0385(9) Uani 1 1 d . . . . .
F6 F 0.8372(4) 0.3047(3) 0.2446(2) 0.0244(6) Uani 1 1 d . . . . .
F5 F 0.5634(4) 0.3029(3) 0.1407(2) 0.0262(6) Uani 1 1 d . . . . .
F2 F 0.8351(4) 0.6101(3) 0.2439(2) 0.0246(6) Uani 1 1 d . . . . .
O2 O 0.8062(5) 0.9920(3) 0.3150(2) 0.0168(5) Uani 1 1 d D . . . .
O1 O 0.8136(5) 0.7722(3) 0.4179(2) 0.0226(6) Uani 1 1 d D . . . .
O3 O 0.8037(6) 1.1961(4) 0.4720(2) 0.0338(7) Uani 1 1 d D . . . .
C2 C 0.8065(6) 1.0347(6) 0.5042(3) 0.0239(8) Uani 1 1 d . . . . .
C1 C 0.8093(6) 0.9282(5) 0.4062(3) 0.0170(7) Uani 1 1 d . . . . .
H2 H 0.804(8) 1.0947(17) 0.312(4) 0.028(12) Uiso 1 1 d D . . . .
H3 H 0.849(7) 1.255(5) 0.516(3) 0.034(16) Uiso 1 1 d D . . . .
H1 H 0.819(8) 0.721(5) 0.363(2) 0.034(14) Uiso 1 1 d D . . . .
H4 H 0.898(6) 1.015(5) 0.551(3) 0.015(12) Uiso 1 1 d . . . . .

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
As1 0.01364(16) 0.01322(15) 0.01530(16) 0.00037(16) 0.00101(16) -0.00012(17)
F3 0.0178(13) 0.0267(14) 0.0322(14) 0.0115(11) 0.0000(11) 0.0072(11)
F4 0.0265(12) 0.0287(11) 0.0198(11) -0.0005(13) 0.0082(10) 0.0017(12)
F7 0.0184(11) 0.0303(11) 0.0182(10) -0.0012(11) 0.0047(9) -0.0029(13)
F1 0.0338(17) 0.056(2) 0.0260(14) -0.0082(13) 0.0116(12) -0.0027(14)
F6 0.0223(15) 0.0206(12) 0.0304(14) 0.0067(11) -0.0010(11) 0.0068(11)
F5 0.0200(14) 0.0277(14) 0.0308(15) -0.0078(11) 0.0020(11) -0.0091(12)
F2 0.0232(15) 0.0206(11) 0.0299(13) -0.0073(10) -0.0003(11) -0.0048(11)
O2 0.0184(12) 0.0157(12) 0.0164(12) 0.0008(10) -0.0006(13) -0.0010(11)
O1 0.0279(16) 0.0205(14) 0.0193(14) 0.0001(12) -0.0029(16) -0.0022(14)
O3 0.049(2) 0.0241(15) 0.0278(17) -0.0129(13) -0.005(2) -0.001(2)
C2 0.0214(19) 0.033(2) 0.0170(17) -0.0070(18) -0.0023(17) 0.003(3)
C1 0.0099(16) 0.0229(19) 0.0183(17) -0.0011(14) 0.0002(15) -0.0020(18)

_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
As1 F5 1.698(3) . ?
As1 F4 1.703(2) . ?
As1 F7 1.716(2) . ?
As1 F3 1.727(2) . ?
As1 F6 1.727(2) . ?
As1 F2 1.754(2) . ?
F1 C2 1.376(5) . ?
O2 C1 1.272(4) . ?
O1 C1 1.258(4) . ?
O3 C2 1.355(5) . ?
C2 C1 1.515(5) . ?

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
F5 As1 F4 91.34(12) . . ?
F5 As1 F7 91.96(12) . . ?
F4 As1 F7 176.70(12) . . ?
F5 As1 F3 90.84(12) . . ?
F4 As1 F3 90.46(12) . . ?
F7 As1 F3 89.64(12) . . ?
F5 As1 F6 90.93(13) . . ?
F4 As1 F6 90.47(12) . . ?
F7 As1 F6 89.34(12) . . ?
F3 As1 F6 177.98(13) . . ?
F5 As1 F2 179.72(14) . . ?
F4 As1 F2 88.92(12) . . ?
F7 As1 F2 87.79(12) . . ?
F3 As1 F2 89.03(13) . . ?
F6 As1 F2 89.19(11) . . ?
O3 C2 F1 111.9(4) . . ?
O3 C2 C1 106.6(3) . . ?
F1 C2 C1 106.1(4) . . ?
O1 C1 O2 120.6(3) . . ?
O1 C1 C2 117.4(3) . . ?
O2 C1 C2 122.0(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 C2 C1 O1 179.5(4) . . . . ?
F1 C2 C1 O1 -61.2(5) . . . . ?
O3 C2 C1 O2 -1.0(6) . . . . ?
F1 C2 C1 O2 118.3(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O2 H2 F6 0.823(13) 1.91(3) 2.669(3) 154(5) 1_565 yes
O3 H3 F3 0.811(13) 2.020(16) 2.826(4) 172(5) 2_675 yes
O1 H1 F2 0.816(13) 1.763(14) 2.579(4) 179(6) . yes
C2 H4 F4 0.92(4) 2.28(4) 3.167(5) 160(3) 4_566 yes

_refine_diff_density_max         0.797
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.119

_shelx_res_file                  
;
TITL shelxt_a.res in P2(1)2(1)2(1)
    shelx.res
    created by SHELXL-2018/3 at 14:53:40 on 24-Oct-2019
CELL  0.71073   7.4858   8.0027  12.7743   90.000   90.000   90.000
ZERR     4.00   0.0003   0.0003   0.0005    0.000    0.000    0.000
LATT  -1
SYMM  1/2 - X, - Y, 1/2 + Z
SYMM  - X, 1/2 + Y, 1/2 - Z
SYMM  1/2 + X, 1/2 - Y, - Z
SFAC  C    H    O    F    AS
UNIT  8 16 12 28 4
MERG   2
TWIN
DFIX 0.82 0.01 O1 H1 O2 H2 O3 H3
EQIV $1 x, y+1, z
HTAB O2 F6_$1
EQIV $2 -x+3/2, -y+2, z+1/2
HTAB O3 F3_$2
HTAB O1 F2
EQIV $3 x+1/2, -y+3/2, -z+1
HTAB C2 F4_$3
FMAP   2
PLAN   20
SIZE     0.150   0.170   0.180
ACTA
HTAB    2.00000
BOND
CONF
LIST   6
L.S.  10
TEMP  -152.00
WGHT    0.024800
BASF   0.49692
FVAR       3.23836
AS1   5    0.696934    0.453879    0.191753    11.00000    0.01364    0.01322 =
         0.01530    0.00037    0.00101   -0.00012
F3    4    0.563044    0.607835    0.138623    11.00000    0.01780    0.02674 =
         0.03224    0.01149   -0.00004    0.00723
F4    4    0.575255    0.457949    0.304390    11.00000    0.02645    0.02869 =
         0.01976   -0.00049    0.00821    0.00171
F7    4    0.827594    0.458172    0.081395    11.00000    0.01839    0.03034 =
         0.01816   -0.00119    0.00468   -0.00290
F1    4    0.653037    0.992011    0.557038    11.00000    0.03375    0.05573 =
         0.02597   -0.00816    0.01160   -0.00271
F6    4    0.837189    0.304661    0.244589    11.00000    0.02230    0.02059 =
         0.03042    0.00668   -0.00101    0.00681
F5    4    0.563371    0.302944    0.140670    11.00000    0.02004    0.02774 =
         0.03083   -0.00776    0.00199   -0.00907
F2    4    0.835108    0.610067    0.243870    11.00000    0.02323    0.02058 =
         0.02989   -0.00726   -0.00033   -0.00480
O2    3    0.806184    0.992047    0.315002    11.00000    0.01836    0.01566 =
         0.01638    0.00076   -0.00062   -0.00100
O1    3    0.813649    0.772185    0.417938    11.00000    0.02792    0.02046 =
         0.01930    0.00008   -0.00288   -0.00216
O3    3    0.803662    1.196086    0.472012    11.00000    0.04942    0.02406 =
         0.02780   -0.01293   -0.00512   -0.00109
C2    1    0.806542    1.034739    0.504184    11.00000    0.02142    0.03328 =
         0.01698   -0.00703   -0.00229    0.00335
C1    1    0.809349    0.928164    0.406156    11.00000    0.00992    0.02293 =
         0.01826   -0.00107    0.00016   -0.00198
H2    2    0.803547    1.094715    0.312372    11.00000    0.02825
H3    2    0.849465    1.255324    0.516025    11.00000    0.03416
H1    2    0.819429    0.720877    0.362813    11.00000    0.03353
H4    2    0.897956    1.014854    0.551214    11.00000    0.01464
HKLF    4




REM  shelxt_a.res in P2(1)2(1)2(1)
REM wR2 = 0.0631, GooF = S = 1.028, Restrained GooF = 1.027 for all data
REM R1 = 0.0320 for 2257 Fo > 4sig(Fo) and 0.0416 for all 2544 data
REM 135 parameters refined using 3 restraints

END

WGHT      0.0248      0.0000

REM Instructions for potential hydrogen bonds
HTAB O2 F6_$1
HTAB O3 F3_$2
HTAB O1 F2
HTAB C2 F4_$3

REM Highest difference peak  0.797,  deepest hole -0.544,  1-sigma level  0.119
Q1    1   0.6970  0.6358  0.1936  11.00000  0.05    0.80
Q2    1   0.6937  0.3447  0.1603  11.00000  0.05    0.56
Q3    1   0.6093  0.5127  0.1372  11.00000  0.05    0.56
Q4    1   0.7026  0.4551  0.4231  11.00000  0.05    0.55
Q5    1   0.8172  0.9627  0.4607  11.00000  0.05    0.54
Q6    1   0.7037  0.3369  0.2108  11.00000  0.05    0.50
Q7    1   0.7781  0.4985  0.2545  11.00000  0.05    0.50
Q8    1   0.7204  0.4572  0.1195  11.00000  0.05    0.49
Q9    1   0.6666  0.4569  0.2598  11.00000  0.05    0.48
Q10   1   0.8026  1.2839  0.4984  11.00000  0.05    0.46
Q11   1   0.7015  0.5567  0.2311  11.00000  0.05    0.46
Q12   1   0.7815  0.3786  0.2498  11.00000  0.05    0.45
Q13   1   0.7083  1.0548  0.5348  11.00000  0.05    0.44
Q14   1   0.7804  0.5594  0.1937  11.00000  0.05    0.44
Q15   1   0.8175  0.5192  0.1235  11.00000  0.05    0.44
Q16   1   0.6178  0.3851  0.2611  11.00000  0.05    0.40
Q17   1   0.6075  0.4069  0.1290  11.00000  0.05    0.40
Q18   1   0.8023  0.2970  0.1984  11.00000  0.05    0.39
Q19   1   0.7520  0.9037  0.4245  11.00000  0.05    0.39
Q20   1   0.8047  0.8783  0.5189  11.00000  0.05    0.39
;
_shelx_res_checksum              76909

_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Heat-sensitive
