# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_PrCNAsF5_TS410
_database_code_depnum_ccdc_archive 'CCDC 1855712'
_audit_update_record             
;
2018-10-02 deposited with the CCDC.
2018-11-14 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C4 H7 As F5 N'
_chemical_formula_sum            'C4 H7 As F5 N'
_chemical_formula_iupac          ?
_chemical_formula_weight         239.03

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

_cell_length_a                   18.521(4)
_cell_length_b                   8.217(2)
_cell_length_c                   5.1493(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     783.7(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7511
_cell_measurement_theta_min      2.2003
_cell_measurement_theta_max      28.3924
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.080
_exptl_crystal_density_diffrn    2.026
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             464

_exptl_absorpt_coefficient_mu    4.363
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker AXS, 2016)'
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_T_max  0.72

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'fine-focus tube'
_diffrn_source_type              ?

_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'

_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega- and phi-scans'

_diffrn_detector_area_resol_mean ?

_diffrn_reflns_number            11247
_diffrn_reflns_av_R_equivalents  0.1164
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_theta_min         2.20
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       6

_refine_special_details          
;
;

_reflns_number_total             964
_reflns_number_gt                729
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0506
_refine_ls_wR_factor_gt          0.0702
_refine_ls_wR_factor_ref         0.0762
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_restrained_S_all      1.109
_refine_ls_number_reflns         964
_refine_ls_number_parameters     71
_refine_ls_number_restraints     54
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0254P)²+0.9555P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.019
_refine_diff_density_min         -0.711
_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'
As As 0.0499 2.0058 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       
'Bruker Instrument Service v2012.12.0.3 (Bruker AXS, 2012)'
_computing_cell_refinement       'APEX3 v2017.3-0 (Bruker AXS, 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS, 2013)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 833)'
_computing_publication_material  'SHELXTL XL 2016/6 (Bruker AXS, 2016)'

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
C C1 0.0469(3) 0.75 0.3173(11) 0.0216(13) Uani d T P S 1 . .
C C2 0.1046(4) 0.751(6) 0.5083(10) 0.0291(17) Uani d . P . 0.5 A -1
H H2A 0.11078 0.640297 0.578987 0.035 Uiso calc U P R 0.5 A -1
H H2AB 0.090744 0.823863 0.653678 0.035 Uiso calc U P R 0.5 A -1
C C3 0.1779(4) 0.8107(10) 0.3920(15) 0.026(2) Uani d . P . 0.5 A -1
H H3A 0.171019 0.916295 0.302788 0.031 Uiso calc U P R 0.5 A -1
H H3AB 0.21355 0.826289 0.533111 0.031 Uiso calc U P R 0.5 A -1
C C4 0.2054(4) 0.6862(11) 0.2024(18) 0.042(3) Uani d . P . 0.5 A -1
H H4A 0.251353 0.72328 0.128817 0.063 Uiso calc U P R 0.5 A -1
H H4B 0.170091 0.671735 0.062544 0.063 Uiso calc U P R 0.5 A -1
H H4C 0.212724 0.582292 0.292116 0.063 Uiso calc U P R 0.5 A -1
As As1 -0.08504(3) 0.75 -0.05245(11) 0.01818(19) Uani d T P S 1 . .
F F1 -0.16005(18) 0.75 -0.2402(7) 0.0296(8) Uani d T P S 1 A .
F F2 -0.11790(13) 0.6030(3) 0.1469(5) 0.0379(7) Uani d . . . 1 . .
F F3 -0.04355(12) 0.6043(3) -0.2360(5) 0.0323(6) Uani d . . . 1 . .
N N1 0.0019(3) 0.75 0.1682(9) 0.0223(11) Uani d T P S 1 A .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
C1 0.020(3) 0.030(3) 0.015(3) 0 0.005(2) 0
C2 0.026(4) 0.052(5) 0.010(3) -0.013(11) -0.005(2) 0.005(15)
C3 0.023(4) 0.036(5) 0.019(5) -0.004(3) -0.003(3) 0.005(3)
C4 0.015(5) 0.077(8) 0.033(5) -0.010(4) 0.002(4) -0.018(5)
As1 0.0132(3) 0.0241(3) 0.0172(3) 0 -0.0019(3) 0
F1 0.0180(17) 0.0391(19) 0.0317(19) 0 -0.0113(14) 0
F2 0.0265(14) 0.0510(16) 0.0363(14) -0.0140(13) -0.0055(12) 0.0199(13)
F3 0.0276(14) 0.0357(14) 0.0336(14) 0.0101(11) -0.0070(11) -0.0140(12)
N1 0.017(3) 0.028(3) 0.022(3) 0 0.000(2) 0

_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
C1 N1 . 1.134(7) ?
C1 C2 . 1.451(8) ?
C2 C3 . 1.562(15) ?
C2 H2A . 0.99 ?
C2 H2AB . 0.99 ?
C3 C4 . 1.503(10) ?
C3 H3A . 0.99 ?
C3 H3AB . 0.99 ?
C4 H4A . 0.98 ?
C4 H4B . 0.98 ?
C4 H4C . 0.98 ?
As1 F1 . 1.693(3) ?
As1 F2 8_575 1.698(2) ?
As1 F2 . 1.698(2) ?
As1 F3 . 1.708(2) ?
As1 F3 8_575 1.708(2) ?
As1 N1 . 1.971(5) ?

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
N1 C1 C2 . . 180.(2) ?
C1 C2 C3 . . 112.5(9) ?
C1 C2 H2A . . 109.1 ?
C3 C2 H2A . . 109.1 ?
C1 C2 H2AB . . 109.1 ?
C3 C2 H2AB . . 109.1 ?
H2A C2 H2AB . . 107.8 ?
C4 C3 C2 . . 109.4(17) ?
C4 C3 H3A . . 109.8 ?
C2 C3 H3A . . 109.8 ?
C4 C3 H3AB . . 109.8 ?
C2 C3 H3AB . . 109.8 ?
H3A C3 H3AB . . 108.3 ?
C3 C4 H4A . . 109.5 ?
C3 C4 H4B . . 109.5 ?
H4A C4 H4B . . 109.5 ?
C3 C4 H4C . . 109.5 ?
H4A C4 H4C . . 109.5 ?
H4B C4 H4C . . 109.5 ?
F1 As1 F2 . 8_575 92.94(12) ?
F1 As1 F2 . . 92.94(12) ?
F2 As1 F2 8_575 . 90.68(19) ?
F1 As1 F3 . . 93.05(12) ?
F2 As1 F3 8_575 . 173.96(12) ?
F2 As1 F3 . . 89.84(13) ?
F1 As1 F3 . 8_575 93.05(12) ?
F2 As1 F3 8_575 8_575 89.84(13) ?
F2 As1 F3 . 8_575 173.96(12) ?
F3 As1 F3 . 8_575 89.02(17) ?
F1 As1 N1 . . 179.64(19) ?
F2 As1 N1 8_575 . 86.81(12) ?
F2 As1 N1 . . 86.81(12) ?
F3 As1 N1 . . 87.21(12) ?
F3 As1 N1 8_575 . 87.21(12) ?
C1 N1 As1 . . 172.5(5) ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C1 C2 C3 C4 . . . . -68.(3) ?

_shelx_res_file                  
;

TITL third_a.res in Pnma
    final.res
    created by SHELXL-2016/6 at 23:00:04 on 01-Oct-2018
CELL  0.71073   18.5210    8.2170    5.1493    90.000    90.000    90.000
ZERR        4    0.0040    0.0020    0.0013     0.000     0.000     0.000
LATT   1
SYMM     0.50000 - X ,            - Y ,    0.50000 + Z
SYMM     0.50000 + X ,    0.50000 - Y ,    0.50000 - Z
SYMM             - X ,    0.50000 + Y ,            - Z
SFAC  C  H As  F  N
UNIT 16 28 4 20 4
SHEL 999 0.77
LIST 4
TEMP  -173
SIZE 0.08 0.09 0.12
L.S. 5
FMAP 2
PLAN 5
ACTA 55
BOND $H
CONF
RIGU
WGHT    0.025400    0.955500
FVAR       0.47280
C1    1    0.046926    0.750000    0.317349    10.50000    0.02014    0.02985 =
         0.01473    0.00000    0.00463    0.00000
PART -1
C2    1    0.104558    0.751452    0.508272    10.50000    0.02595    0.05180 =
         0.00960    0.00507   -0.00483   -0.01262
AFIX  23
H2A   2    0.110780    0.640297    0.578987    10.50000   -1.20000
H2AB  2    0.090744    0.823863    0.653678    10.50000   -1.20000
AFIX   0
C3    1    0.177909    0.810707    0.392002    10.50000    0.02284    0.03640 =
         0.01944    0.00495   -0.00322   -0.00430
AFIX  23
H3A   2    0.171019    0.916295    0.302788    10.50000   -1.20000
H3AB  2    0.213550    0.826289    0.533111    10.50000   -1.20000
AFIX   0
C4    1    0.205413    0.686163    0.202363    10.50000    0.01549    0.07677 =
         0.03282   -0.01830    0.00155   -0.01048
AFIX 137
H4A   2    0.251353    0.723280    0.128817    10.50000   -1.50000
H4B   2    0.170091    0.671735    0.062544    10.50000   -1.50000
H4C   2    0.212724    0.582292    0.292116    10.50000   -1.50000
AFIX   0
PART 0
AS1   3   -0.085043    0.750000   -0.052453    10.50000    0.01323    0.02408 =
         0.01724    0.00000   -0.00193    0.00000
F1    4   -0.160051    0.750000   -0.240223    10.50000    0.01798    0.03908 =
         0.03170    0.00000   -0.01128    0.00000
F2    4   -0.117899    0.603023    0.146940    11.00000    0.02654    0.05097 =
         0.03626    0.01992   -0.00549   -0.01400
F3    4   -0.043548    0.604251   -0.236038    11.00000    0.02756    0.03568 =
         0.03359   -0.01397   -0.00702    0.01007
N1    5    0.001913    0.750000    0.168151    10.50000    0.01663    0.02804 =
         0.02221    0.00000   -0.00045    0.00000
HKLF 4 1 0.0000 0.0000 1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000




REM  third_a.res in Pnma
REM R1 =  0.0506 for     729 Fo > 4sig(Fo)  and  0.0795 for all     964 data
REM     71 parameters refined using     54 restraints

END

WGHT      0.0261      0.8497

REM Highest difference peak  1.019,  deepest hole -0.711,  1-sigma level  0.127
Q1    1  -0.0724  0.7500 -0.2335  10.50000  0.05    1.02
Q2    1  -0.1082  0.7500  0.1055  10.50000  0.05    0.78
Q3    1  -0.0618  0.7500  0.1041  10.50000  0.05    0.72
Q4    1  -0.1358  0.6480 -0.0215  11.00000  0.05    0.55
Q5    1  -0.0277  0.7500  0.0400  10.50000  0.05    0.53
;
_shelx_res_checksum              13287
####################################################################### 
# 
# 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_I
_database_code_depnum_ccdc_archive 'CCDC 1855713'
_audit_update_record             
;
2018-07-13 deposited with the CCDC.
2018-11-14 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C H F5 N Sb'
_chemical_formula_sum            'C H F5 N Sb'
_chemical_formula_iupac          ?
_chemical_formula_weight         243.78

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   6.2721(13)
_cell_length_b                   8.1472(17)
_cell_length_c                   10.157(2)
_cell_angle_alpha                90
_cell_angle_beta                 95.375(4)
_cell_angle_gamma                90
_cell_volume                     516.74(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6811
_cell_measurement_theta_min      3.2104
_cell_measurement_theta_max      30.4317
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       plate
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_size_max          0.217
_exptl_crystal_size_mid          0.189
_exptl_crystal_size_min          0.052
_exptl_crystal_density_diffrn    3.134
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             440

_exptl_absorpt_coefficient_mu    5.348
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5 (Bruker AXS, 2014)'
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_T_max  0.77

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'fine-focus tube'
_diffrn_source_type              ?

_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'

_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega- and phi-scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            1543
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_theta_min         3.21
_diffrn_reflns_theta_max         30.43
_diffrn_reflns_theta_full        30.43
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14

_refine_special_details          
;
;

_reflns_number_total             1543
_reflns_number_gt                1434
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0224
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0580
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_restrained_S_all      1.109
_refine_ls_number_reflns         1543
_refine_ls_number_parameters     76
_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)+(0.0262P)²+0.5137P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.655
_refine_diff_density_min         -1.020
_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'
N N 0.0061 0.0033 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       
'Bruker Instrument Service v2012.12.0.3 (Bruker AXS, 2012)'
_computing_cell_refinement       'APEX2 v2014.11-0 (Bruker AXS, 2014)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS, 2013)'
_computing_structure_solution    'SHELXTL XT 2014/4 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXTL XL 2014/7 (Bruker AXS, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXTL XT 2014/4 (Bruker AXS, 2014)'

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
C C1 0.6421(5) 0.2651(3) 0.4458(3) 0.0155(5) Uani d . . . 1 . .
H H1 0.752(6) 0.241(4) 0.507(3) 0.019 Uiso d U . . 1 . .
N N1 0.5037(4) 0.3030(3) 0.3737(3) 0.0152(5) Uani d . . . 1 . .
F F1 -0.0271(3) 0.3857(2) 0.13287(18) 0.0188(4) Uani d . . . 1 . .
F F2 0.0711(3) 0.2746(2) 0.38204(18) 0.0203(4) Uani d . . . 1 . .
F F3 0.2530(3) 0.1326(2) 0.18482(19) 0.0196(4) Uani d . . . 1 . .
F F4 0.4016(3) 0.4190(2) 0.11873(17) 0.0181(4) Uani d . . . 1 . .
F F5 0.2286(3) 0.5584(2) 0.31426(18) 0.0189(4) Uani d . . . 1 . .
Sb Sb1 0.22230(3) 0.34653(2) 0.24369(2) 0.01044(7) Uani d . . . 1 . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
C1 0.0154(13) 0.0167(12) 0.0144(13) -0.0004(10) 0.0010(11) -0.0027(10)
N1 0.0155(12) 0.0133(10) 0.0169(11) -0.0002(9) 0.0018(9) -0.0009(9)
F1 0.0167(9) 0.0179(8) 0.0201(9) 0.0020(7) -0.0066(7) -0.0020(7)
F2 0.0161(9) 0.0279(9) 0.0175(8) -0.0038(7) 0.0054(7) 0.0040(7)
F3 0.0215(10) 0.0116(7) 0.0251(10) 0.0011(6) -0.0007(8) -0.0049(7)
F4 0.0215(9) 0.0186(8) 0.0151(8) -0.0035(7) 0.0062(7) 0.0005(6)
F5 0.0204(9) 0.0142(8) 0.0214(9) 0.0012(6) -0.0017(7) -0.0056(6)
Sb1 0.01064(11) 0.01055(11) 0.01001(11) -0.00031(5) 0.00037(7) -0.00064(5)

_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
C1 N1 . 1.125(4) ?
C1 H1 . 0.91(4) ?
N1 Sb1 . 2.132(3) ?
F1 Sb1 . 1.8673(18) ?
F2 Sb1 . 1.8620(17) ?
F3 Sb1 . 1.8585(17) ?
F4 Sb1 . 1.8686(17) ?
F5 Sb1 . 1.8679(17) ?

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
N1 C1 H1 . . 176.(2) ?
C1 N1 Sb1 . . 172.7(3) ?
F3 Sb1 F2 . . 91.32(8) ?
F3 Sb1 F1 . . 94.17(8) ?
F2 Sb1 F1 . . 92.96(8) ?
F3 Sb1 F5 . . 172.27(9) ?
F2 Sb1 F5 . . 89.73(8) ?
F1 Sb1 F5 . . 93.42(8) ?
F3 Sb1 F4 . . 89.46(8) ?
F2 Sb1 F4 . . 173.48(8) ?
F1 Sb1 F4 . . 93.44(8) ?
F5 Sb1 F4 . . 88.64(8) ?
F3 Sb1 N1 . . 86.48(9) ?
F2 Sb1 N1 . . 86.04(9) ?
F1 Sb1 N1 . . 178.82(8) ?
F5 Sb1 N1 . . 85.96(9) ?
F4 Sb1 N1 . . 87.55(9) ?

_shelx_res_file                  
;
TITL twin4_a.res in P2(1)/c
CELL  0.71073   6.2721   8.1472  10.1568   90.000   95.375   90.000
ZERR    4.000   0.0013   0.0017   0.0022    0.000    0.004    0.000
LATT 1
SYMM -X, 1/2+Y, 1/2-Z
SFAC C  H  N  F  Sb
UNIT 4 4 4 20 4
LIST 4
L.S. 10
FMAP 2
PLAN 4
ACTA 58
BOND $H
CONF
SIZE 0.052 0.189 0.217
TEMP -173.150
WGHT    0.026200    0.513700
FVAR       0.43277
C1    1    0.642093    0.265084    0.445754    11.00000    0.01541    0.01672 =
         0.01444   -0.00270    0.00096   -0.00036
H1    2    0.752311    0.241265    0.507212    11.00000   -1.20000
N1    3    0.503661    0.303016    0.373680    11.00000    0.01550    0.01332 =
         0.01693   -0.00090    0.00183   -0.00022
F1    4   -0.027132    0.385744    0.132866    11.00000    0.01672    0.01789 =
         0.02013   -0.00198   -0.00660    0.00201
F2    4    0.071095    0.274588    0.382040    11.00000    0.01615    0.02786 =
         0.01751    0.00403    0.00540   -0.00376
F3    4    0.252992    0.132588    0.184824    11.00000    0.02153    0.01161 =
         0.02506   -0.00490   -0.00070    0.00106
F4    4    0.401600    0.418972    0.118727    11.00000    0.02151    0.01858 =
         0.01512    0.00048    0.00623   -0.00352
F5    4    0.228611    0.558382    0.314257    11.00000    0.02038    0.01418 =
         0.02140   -0.00563   -0.00165    0.00115
SB1   5    0.222295    0.346526    0.243693    11.00000    0.01064    0.01055 =
         0.01001   -0.00064    0.00037   -0.00031
HKLF 4

REM  twin4_a.res in P2(1)/c
REM R1 =  0.0224 for    1434 Fo > 4sig(Fo)  and  0.0251 for all    1543 data
REM     76 parameters refined using      0 restraints

END

WGHT      0.0262      0.5137

REM Highest difference peak  0.655,  deepest hole -1.020,  1-sigma level  0.179
Q1    1  -0.0839  0.3440  0.2978  11.00000  0.05    0.66
Q2    1   0.3778  0.3584  0.1735  11.00000  0.05    0.65
Q3    1   0.4936  0.5424  0.1129  11.00000  0.05    0.55
Q4    1   0.5511  0.3715  0.3009  11.00000  0.05    0.55
;
_shelx_res_checksum              42056
####################################################################### 
# 
# 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_HCNAsF5
_database_code_depnum_ccdc_archive 'CCDC 1855714'
_audit_update_record             
;
2018-10-02 deposited with the CCDC.
2018-11-14 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            AsF5HCN
_chemical_formula_moiety         'C H As F5 N'
_chemical_formula_sum            'C H As F5 N'
_chemical_formula_iupac          ?
_chemical_formula_weight         196.95
_chemical_absolute_configuration ?

_chemical_melting_point          ?

_space_group_crystal_system      tetragonal
_space_group_name_H-M_alt        'P 41 21 2'
_space_group_name_Hall           'P 4abw 2nw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+1/4'
'y+1/2, -x+1/2, z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'x+1/2, -y+1/2, -z+3/4'
'y, x, -z'
'-y, -x, -z+1/2'

_cell_length_a                   5.4973(15)
_cell_length_b                   5.4973(15)
_cell_length_c                   16.475(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     497.9(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5287
_cell_measurement_theta_min      2.4726
_cell_measurement_theta_max      30.4454
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.338
_exptl_crystal_size_mid          0.232
_exptl_crystal_size_min          0.176
_exptl_crystal_density_diffrn    2.628
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             368

_exptl_absorpt_coefficient_mu    6.836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker AXS, 2016)'
_exptl_absorpt_correction_T_min  0.29
_exptl_absorpt_correction_T_max  0.38

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'fine-focus tube'
_diffrn_source_type              ?

_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'

_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega- and phi-scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            12048
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_theta_min         3.91
_diffrn_reflns_theta_max         30.57
_diffrn_reflns_theta_full        30.57
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23

_refine_special_details          
;

Refined as a 2-component inversion twin.
;

_reflns_number_total             762
_reflns_number_gt                673
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0246
_refine_ls_wR_factor_gt          0.0552
_refine_ls_wR_factor_ref         0.0567
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_restrained_S_all      1.198
_refine_ls_number_reflns         762
_refine_ls_number_parameters     41
_refine_ls_number_restraints     1
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0167P)²+0.5235P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.472
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;

Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(7)

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'
As As 0.0499 2.0058 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       
'Bruker Instrument Service v2012.12.0.3 (Bruker AXS, 2012)'
_computing_cell_refinement       'APEX3 v2018.1-0 (Bruker AXS, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS, 2013)'
_computing_structure_solution    'SHELXTL XT 2014/5 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXTL XL 2017/1 (Bruker AXS, 2017)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 882)'
_computing_publication_material  'SHELXTL XL 2017/1 (Bruker AXS, 2017)'

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
C C1 0.1026(5) 0.8974(5) 0.25 0.0236(8) Uani d T P DS 1 . .
H H1 -0.025(3) 1.025(3) 0.25 0.028 Uiso d U P DS 1 . .
As As1 0.50372(5) 0.49628(5) 0.25 0.01659(13) Uani d T P S 1 . .
F F1 0.3572(5) 0.3663(4) 0.33001(11) 0.0318(4) Uani d . . . 1 . .
F F2 0.3184(4) 0.3431(4) 0.18455(11) 0.0309(4) Uani d . . . 1 . .
F F3 0.7239(3) 0.2761(3) 0.25 0.0390(8) Uani d T P S 1 . .
N N1 0.2487(4) 0.7513(4) 0.25 0.0179(6) Uani d T P S 1 . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
C1 0.0202(11) 0.0202(11) 0.030(2) 0.0004(15) 0.0025(14) 0.0025(14)
As1 0.01828(15) 0.01828(15) 0.01320(19) 0.00657(12) 0.00090(10) 0.00090(10)
F1 0.0358(12) 0.0329(12) 0.0266(8) 0.0063(9) 0.0078(9) 0.0138(9)
F2 0.0378(14) 0.0254(11) 0.0296(9) 0.0044(8) -0.0076(9) -0.0120(9)
F3 0.0444(12) 0.0444(12) 0.0283(14) 0.0329(15) 0.0060(15) 0.0060(15)
N1 0.0176(9) 0.0176(9) 0.0184(15) 0.0011(12) -0.0004(14) -0.0004(14)

_geom_special_details            
;

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 N1 . 1.136(5) ?
C1 H1 . 1.00(2) ?
As1 F1 . 1.7020(17) ?
As1 F1 8_665 1.7021(17) ?
As1 F2 8_665 1.7058(18) ?
As1 F2 . 1.7058(18) ?
As1 F3 . 1.712(2) ?
As1 N1 . 1.983(3) ?

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
N1 C1 H1 . . 180.0 ?
F1 As1 F1 . 8_665 175.7(2) ?
F1 As1 F2 . 8_665 89.70(10) ?
F1 As1 F2 8_665 8_665 89.98(10) ?
F1 As1 F2 . . 89.98(10) ?
F1 As1 F2 8_665 . 89.70(10) ?
F2 As1 F2 8_665 . 171.60(17) ?
F1 As1 F3 . . 92.17(10) ?
F1 As1 F3 8_665 . 92.17(10) ?
F2 As1 F3 8_665 . 94.20(9) ?
F2 As1 F3 . . 94.20(9) ?
F1 As1 N1 . . 87.83(10) ?
F1 As1 N1 8_665 . 87.83(10) ?
F2 As1 N1 8_665 . 85.80(9) ?
F2 As1 N1 . . 85.80(9) ?
F3 As1 N1 . . 180.00(2) ?
C1 N1 As1 . . 180.0(2) ?

_shelx_res_file                  
;

TITL final in P4(3)2(1)2
    final.res
    created by SHELXL-2017/1 at 11:17:01 on 01-Oct-2018
CELL 0.71073   5.49730   5.49730  16.47470  90.0000  90.0000  90.0000
ZERR    4.00   0.00150   0.00150   0.00460   0.0000   0.0000   0.0000
LATT -1
SYMM  -x, -y, 1/2+z
SYMM  1/2-y, 1/2+x, 1/4+z
SYMM  1/2+y, 1/2-x, 3/4+z
SYMM  1/2-x, 1/2+y, 1/4-z
SYMM  1/2+x, 1/2-y, 3/4-z
SYMM  +y, +x, -z
SYMM  -y, -x, 1/2-z
SFAC C H AS F N
UNIT 4 4 4 20 4
TEMP -173.150
SIZE 0.176 0.232 0.338
L.S. 10
ACTA 58
BOND $H
LIST 4
FMAP 2
DFIX 0.95 C1 H1
PLAN 5
TWIN
WGHT    0.016700    0.523500
BASF   0.48647
FVAR       0.18416
C1    1    0.102598    0.897402    0.250000    10.50000    0.02018    0.02018 =
         0.03035    0.00247    0.00247    0.00038
H1    2   -0.025440    1.025440    0.250000    10.50000   -1.20000
AS1   3    0.503716    0.496284    0.250000    10.50000    0.01828    0.01828 =
         0.01320    0.00090    0.00090    0.00657
F1    4    0.357194    0.366317    0.330014    11.00000    0.03580    0.03295 =
         0.02662    0.01382    0.00778    0.00628
F2    4    0.318380    0.343098    0.184554    11.00000    0.03778    0.02541 =
         0.02955   -0.01202   -0.00759    0.00439
F3    4    0.723948    0.276052    0.250000    10.50000    0.04435    0.04435 =
         0.02828    0.00600    0.00600    0.03294
N1    5    0.248689    0.751311    0.250000    10.50000    0.01763    0.01763 =
         0.01845   -0.00044   -0.00044    0.00113
HKLF 4




REM  final in P4(3)2(1)2
REM R1 =  0.0246 for     673 Fo > 4sig(Fo)  and  0.0288 for all     762 data
REM     41 parameters refined using      1 restraints

END

WGHT      0.0159      0.5646

REM Highest difference peak  0.329,  deepest hole -0.472,  1-sigma level  0.089
Q1    1  -0.1493  1.1493  0.2500  10.50000  0.05    0.33
Q2    1   0.3787  0.2345  0.3096  11.00000  0.05    0.26
Q3    1   0.3917  0.4034  0.1493  11.00000  0.05    0.24
Q4    1   0.9989  0.3586  0.3175  11.00000  0.05    0.24
Q5    1  -0.0256  1.1617  0.3212  11.00000  0.05    0.21
;
_shelx_res_checksum              78754
####################################################################### 
# 
# 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_PrCNSbF5_AN30
_database_code_depnum_ccdc_archive 'CCDC 1855715'
_audit_update_record             
;
2018-10-02 deposited with the CCDC.
2018-11-14 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C4 H7 F5 N Sb'
_chemical_formula_sum            'C4 H7 F5 N Sb'
_chemical_formula_iupac          ?
_chemical_formula_weight         285.86

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

_cell_length_a                   18.894(7)
_cell_length_b                   8.416(3)
_cell_length_c                   5.261(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     836.6(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    95
_cell_measurement_theta_min      6.43
_cell_measurement_theta_max      48.01
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.079
_exptl_crystal_density_diffrn    2.270
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             536

_exptl_absorpt_coefficient_mu    3.322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker AXS, 2016)'
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_T_max  0.78

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'fine-focus tube'
_diffrn_source_type              ?

_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'

_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega- and phi-scans'

_diffrn_detector_area_resol_mean ?

_diffrn_reflns_number            17084
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_theta_min         2.16
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_full        28.27
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7

_refine_special_details          
;
;

_reflns_number_total             1101
_reflns_number_gt                949
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0167
_refine_ls_wR_factor_gt          0.0335
_refine_ls_wR_factor_ref         0.0347
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_number_reflns         1101
_refine_ls_number_parameters     71
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0173P)²+0.1605P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.594
_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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       
'Bruker Instrument Service v2012.12.0.3 (Bruker AXS, 2012)'
_computing_cell_refinement       'APEX3 v2017.3-0 (Bruker AXS, 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS, 2013)'
_computing_structure_solution    'SHELXTL XT 2014/5 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXTL XL 2016/6 (Bruker AXS, 2016)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 833)'
_computing_publication_material  'SHELXTL XL 2016/6 (Bruker AXS, 2016)'

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
Sb Sb1 -0.08798(2) 0.25 -0.05072(4) 0.01793(6) Uani d T P S 1 . .
F F1 -0.16918(8) 0.25 -0.2507(3) 0.0305(4) Uani d T P S 1 . .
F F2 -0.04339(6) 0.40483(15) -0.2495(2) 0.0330(3) Uani d . . . 1 . .
F F4 -0.12264(7) 0.09143(16) 0.1631(3) 0.0396(3) Uani d . . . 1 . .
N N1 0.00348(12) 0.25 0.1796(5) 0.0235(5) Uani d T P S 1 A .
C C1 0.04749(14) 0.25 0.3268(6) 0.0227(6) Uani d T P S 1 . .
C C2 0.10385(16) 0.2494(19) 0.5169(7) 0.0325(11) Uani d . P . 0.5 A -1
H H2A 0.090371 0.178377 0.658876 0.039 Uiso calc U P R 0.5 A -1
H H2AB 0.109744 0.357984 0.586199 0.039 Uiso calc U P R 0.5 A -1
C C3 0.1759(2) 0.1918(5) 0.4005(8) 0.0262(10) Uani d . P . 0.5 A -1
H H3A 0.211182 0.176729 0.537636 0.031 Uiso calc U P R 0.5 A -1
H H3AB 0.169131 0.088769 0.313134 0.031 Uiso calc U P R 0.5 A -1
C C4 0.2025(2) 0.3149(6) 0.2128(9) 0.0457(14) Uani d . P . 0.5 A -1
H H4A 0.247978 0.280133 0.142184 0.069 Uiso calc U P R 0.5 A -1
H H4B 0.208795 0.416862 0.299944 0.069 Uiso calc U P R 0.5 A -1
H H4C 0.168073 0.327218 0.075048 0.069 Uiso calc U P R 0.5 A -1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Sb1 0.01406(9) 0.02218(10) 0.01754(10) 0 -0.00111(8) 0
F1 0.0197(9) 0.0421(10) 0.0298(10) 0 -0.0091(7) 0
F2 0.0329(7) 0.0348(7) 0.0314(7) -0.0110(5) -0.0044(6) 0.0128(6)
F4 0.0314(7) 0.0497(8) 0.0378(8) -0.0158(6) -0.0058(6) 0.0205(7)
N1 0.0180(12) 0.0292(13) 0.0231(14) 0 -0.0030(10) 0
C1 0.0174(14) 0.0264(15) 0.0244(17) 0 0.0038(12) 0
C2 0.0216(16) 0.056(3) 0.020(2) 0.003(8) -0.0043(14) -0.024(7)
C3 0.0182(18) 0.034(2) 0.027(3) 0.0032(15) -0.0060(17) -0.0059(16)
C4 0.024(2) 0.079(4) 0.034(3) 0.004(2) 0.003(2) 0.019(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
Sb1 F1 . 1.8602(16) ?
Sb1 F4 8_565 1.8643(13) ?
Sb1 F4 . 1.8643(13) ?
Sb1 F2 8_565 1.8712(12) ?
Sb1 F2 . 1.8712(12) ?
Sb1 N1 . 2.111(2) ?
N1 C1 . 1.136(4) ?
C1 C2 . 1.461(4) ?
C2 C3 . 1.570(6) ?
C2 H2A . 0.99 ?
C2 H2AB . 0.99 ?
C3 C4 . 1.517(6) ?
C3 H3A . 0.99 ?
C3 H3AB . 0.99 ?
C4 H4A . 0.98 ?
C4 H4B . 0.98 ?
C4 H4C . 0.98 ?

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
F1 Sb1 F4 . 8_565 92.96(6) ?
F1 Sb1 F4 . . 92.96(6) ?
F4 Sb1 F4 8_565 . 91.43(10) ?
F1 Sb1 F2 . 8_565 93.17(6) ?
F4 Sb1 F2 8_565 8_565 173.67(5) ?
F4 Sb1 F2 . 8_565 89.82(7) ?
F1 Sb1 F2 . . 93.17(6) ?
F4 Sb1 F2 8_565 . 89.82(7) ?
F4 Sb1 F2 . . 173.67(5) ?
F2 Sb1 F2 8_565 . 88.28(9) ?
F1 Sb1 N1 . . 179.40(9) ?
F4 Sb1 N1 8_565 . 86.62(6) ?
F4 Sb1 N1 . . 86.62(6) ?
F2 Sb1 N1 8_565 . 87.26(6) ?
F2 Sb1 N1 . . 87.26(6) ?
C1 N1 Sb1 . . 172.1(2) ?
N1 C1 C2 . . 179.7(6) ?
C1 C2 C3 . . 111.5(3) ?
C1 C2 H2A . . 109.3 ?
C3 C2 H2A . . 109.3 ?
C1 C2 H2AB . . 109.3 ?
C3 C2 H2AB . . 109.3 ?
H2A C2 H2AB . . 108.0 ?
C4 C3 C2 . . 109.3(6) ?
C4 C3 H3A . . 109.8 ?
C2 C3 H3A . . 109.8 ?
C4 C3 H3AB . . 109.8 ?
C2 C3 H3AB . . 109.8 ?
H3A C3 H3AB . . 108.3 ?
C3 C4 H4A . . 109.5 ?
C3 C4 H4B . . 109.5 ?
H4A C4 H4B . . 109.5 ?
C3 C4 H4C . . 109.5 ?
H4A C4 H4C . . 109.5 ?
H4B C4 H4C . . 109.5 ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C1 C2 C3 C4 . . . . 68.1(10) ?

_shelx_res_file                  
;

TITL final_a.res in Pnma
    final_a.res
    created by SHELXL-2016/6 at 22:41:13 on 01-Oct-2018
CELL  0.71073   18.8940    8.4160    5.2610    90.000    90.000    90.000
ZERR        4    0.0070    0.0030    0.0020     0.000     0.000     0.000
LATT   1
SYMM     0.50000 - X ,            - Y ,    0.50000 + Z
SYMM     0.50000 + X ,    0.50000 - Y ,    0.50000 - Z
SYMM             - X ,    0.50000 + Y ,            - Z
SFAC  C  H  F  N Sb
UNIT 16 28 20 4 4
SHEL 999 0.75
LIST 4
TEMP  -173
L.S. 5
FMAP 2
PLAN -20
ACTA 55
SIZE 0.079 0.093 0.149
BOND $H
CONF
WGHT    0.017300    0.160500
FVAR       0.37700
RESI 0
SB1   5   -0.087982    0.250000   -0.050716    10.50000    0.01406    0.02218 =
         0.01754    0.00000   -0.00111    0.00000
F1    3   -0.169177    0.250000   -0.250703    10.50000    0.01968    0.04210 =
         0.02979    0.00000   -0.00908    0.00000
F2    3   -0.043386    0.404835   -0.249459    11.00000    0.03287    0.03478 =
         0.03136    0.01277   -0.00441   -0.01097
F4    3   -0.122643    0.091429    0.163125    11.00000    0.03142    0.04965 =
         0.03781    0.02050   -0.00582   -0.01580
N1    4    0.003481    0.250000    0.179642    10.50000    0.01804    0.02923 =
         0.02310    0.00000   -0.00305    0.00000
C1    1    0.047493    0.250000    0.326846    10.50000    0.01742    0.02636 =
         0.02439    0.00000    0.00380    0.00000
PART   -1
C2    1    0.103849    0.249418    0.516915    10.50000    0.02156    0.05551 =
         0.02046   -0.02363   -0.00431    0.00292
AFIX  23
H2A   2    0.090371    0.178377    0.658876    10.50000   -1.20000
H2AB  2    0.109744    0.357984    0.586199    10.50000   -1.20000
AFIX   0
C3    1    0.175933    0.191825    0.400515    10.50000    0.01819    0.03369 =
         0.02677   -0.00588   -0.00604    0.00322
AFIX  23
H3A   2    0.211182    0.176729    0.537636    10.50000   -1.20000
H3AB  2    0.169131    0.088769    0.313134    10.50000   -1.20000
AFIX   0
C4    1    0.202550    0.314900    0.212814    10.50000    0.02425    0.07895 =
         0.03385    0.01884    0.00260    0.00366
AFIX 137
H4A   2    0.247978    0.280133    0.142184    10.50000   -1.50000
H4B   2    0.208795    0.416862    0.299944    10.50000   -1.50000
H4C   2    0.168073    0.327218    0.075048    10.50000   -1.50000
AFIX   0
HKLF 4 1 0.0000 0.0000 1.0000 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000




REM  final_a.res in Pnma
REM R1 =  0.0167 for     949 Fo > 4sig(Fo)  and  0.0239 for all    1101 data
REM     71 parameters refined using      0 restraints

END

WGHT      0.0173      0.1605

REM Highest difference peak  0.414,  deepest hole -0.594,  1-sigma level  0.081
Q1    1  -0.0397  0.2500  0.0859  10.50000  0.05    0.41
Q2    1  -0.0465  0.2500 -0.0576  10.50000  0.05    0.40
Q3    1  -0.2641  0.2500 -0.3523  10.50000  0.05    0.35
Q4    1  -0.0870  0.1669  0.0926  11.00000  0.05    0.35
Q5    1  -0.1255  0.2500 -0.2435  10.50000  0.05    0.33
Q6    1   0.0610  0.2500  0.5361  10.50000  0.05    0.32
Q7    1  -0.0033  0.2500  0.2540  10.50000  0.05    0.31
Q8    1  -0.1360  0.2500  0.0505  10.50000  0.05    0.31
Q9    1  -0.0700  0.1797 -0.1772  11.00000  0.05    0.31
Q10   1  -0.1359  0.2239 -0.1002  11.00000  0.05    0.30
Q11   1   0.1479  0.2500  0.4842  10.50000  0.05    0.29
Q12   1   0.1287  0.2500 -0.0095  10.50000  0.05    0.28
Q13   1  -0.2297  0.2500 -0.1613  10.50000  0.05    0.27
Q14   1   0.2233  0.2500  0.1429  10.50000  0.05    0.27
Q15   1   0.1843  0.2500  0.2984  10.50000  0.05    0.27
Q16   1   0.0487  0.2500  0.1754  10.50000  0.05    0.26
Q17   1   0.1789  0.2500  0.0859  10.50000  0.05    0.24
Q18   1  -0.1826  0.2500 -0.0254  10.50000  0.05    0.24
Q19   1   0.2466  0.2500  0.0827  10.50000  0.05    0.24
Q20   1  -0.0021  0.1735  0.1168  11.00000  0.05    0.22
;
_shelx_res_checksum              56996
####################################################################### 
# 
# 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_TS377
_database_code_depnum_ccdc_archive 'CCDC 1855718'
_audit_update_record             
;
2018-07-13 deposited with the CCDC.
2018-11-14 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C10 H18 F10 N2 Sb2'
_chemical_formula_sum            'C10 H18 F10 N2 Sb2'
_chemical_formula_iupac          ?
_chemical_formula_weight         599.76

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/m 1'
_space_group_name_Hall           '-P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   5.970(3)
_cell_length_b                   8.897(5)
_cell_length_c                   9.201(5)
_cell_angle_alpha                90
_cell_angle_beta                 97.380(8)
_cell_angle_gamma                90
_cell_volume                     484.7(4)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    3980
_cell_measurement_theta_min      2.2319
_cell_measurement_theta_max      28.2423
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.064
_exptl_crystal_density_diffrn    2.055
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             284

_exptl_absorpt_coefficient_mu    2.872
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   'TWINABS 2012/1 (Bruker AXS, 2014)'
_exptl_absorpt_correction_T_min  0.540353
_exptl_absorpt_correction_T_max  0.746069

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'fine-focus tube'
_diffrn_source_type              ?

_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'

_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega- and phi-scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            1532
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_theta_min         2.23
_diffrn_reflns_theta_max         30.44
_diffrn_reflns_theta_full        30.44
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.983
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       13

_refine_special_details          
;

Refined as a 2-component twin.
;

_reflns_number_total             1532
_reflns_number_gt                1334
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0398
_refine_ls_wR_factor_gt          0.0715
_refine_ls_wR_factor_ref         0.0826
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.067
_refine_ls_number_reflns         1532
_refine_ls_number_parameters     70
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0186P)²+2.7268P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.292
_refine_diff_density_min         -2.683
_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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       
'Bruker Instrument Service v2012.12.0.3 (Bruker AXS, 2012)'
_computing_cell_refinement       'APEX2 v2014.11-0 (Bruker AXS, 2014)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS, 2013)'
_computing_structure_solution    'SHELXTL XT 2014/4 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 807)'
_computing_publication_material  'SHELXTL XT 2014/4 (Bruker AXS, 2014)'

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
C C1 0.7897(12) 0.25 0.6316(7) 0.0184(13) Uani d T P S 1 . .
C C2 0.9324(12) 0.25 0.7744(8) 0.0202(14) Uani d T P S 1 . .
C C3 1.0797(10) 0.3919(6) 0.7836(6) 0.0273(11) Uani d . . . 1 . .
H H3A 1.1734 0.3914 0.7036 0.041 Uiso calc U . R 1 . .
H H3B 1.1771 0.3937 0.8778 0.041 Uiso calc U . R 1 . .
H H3C 0.9827 0.4811 0.7753 0.041 Uiso calc U . R 1 . .
C C4 0.7722(14) 0.25 0.8941(8) 0.0285(17) Uani d T P S 1 . .
H H4A 0.6573 0.3282 0.8721 0.043 Uiso calc U P R 0.5 . .
H H4B 0.8595 0.2701 0.9897 0.043 Uiso calc U P R 0.5 . .
H H4C 0.6986 0.1517 0.8961 0.043 Uiso calc U P R 0.5 . .
F F1 0.2530(9) 0.25 0.1500(5) 0.0342(11) Uani d T P S 1 . .
F F2 0.2159(8) 0.25 0.4419(4) 0.0307(10) Uani d T P S 1 . .
F F3 0.7060(8) 0.25 0.2279(4) 0.0294(10) Uani d T P S 1 . .
F F4 0.4569(6) 0.4597(3) 0.3316(3) 0.0286(6) Uani d . . . 1 . .
N N1 0.6755(10) 0.25 0.5210(6) 0.0186(12) Uani d T P S 1 . .
Sb Sb1 0.45059(9) 0.25 0.32521(5) 0.01680(12) Uani d T P S 1 . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
C1 0.018(3) 0.018(3) 0.020(3) 0 0.004(3) 0
C2 0.018(3) 0.026(4) 0.016(3) 0 -0.003(3) 0
C3 0.024(3) 0.026(2) 0.031(2) -0.004(2) -0.003(2) 0.000(2)
C4 0.024(4) 0.040(5) 0.022(3) 0 0.003(3) 0
F1 0.033(3) 0.042(3) 0.023(2) 0 -0.013(2) 0
F2 0.022(2) 0.045(3) 0.026(2) 0 0.006(2) 0
F3 0.030(3) 0.040(3) 0.021(2) 0 0.0113(19) 0
F4 0.0357(15) 0.0173(12) 0.0311(14) 0.0031(15) -0.0027(16) 0.0015(12)
N1 0.018(3) 0.021(3) 0.016(3) 0 -0.003(2) 0
Sb1 0.0186(2) 0.01707(19) 0.01429(18) 0 0.00030(18) 0

_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
C1 N1 . 1.150(8) ?
C1 C2 . 1.471(9) ?
C2 C3 . 1.535(7) ?
C2 C3 4_565 1.535(7) ?
C2 C4 . 1.548(10) ?
C3 H3A . 0.98 ?
C3 H3B . 0.98 ?
C3 H3C . 0.98 ?
C4 H4A . 0.98 ?
C4 H4B . 0.98 ?
C4 H4C . 0.98 ?
F1 Sb1 . 1.871(4) ?
F2 Sb1 . 1.871(5) ?
F3 Sb1 . 1.865(5) ?
F4 Sb1 . 1.867(3) ?
N1 Sb1 . 2.104(6) ?
Sb1 F4 4_565 1.867(3) ?

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
N1 C1 C2 . . 179.1(7) ?
C1 C2 C3 . . 108.1(4) ?
C1 C2 C3 . 4_565 108.1(4) ?
C3 C2 C3 . 4_565 110.7(6) ?
C1 C2 C4 . . 107.2(6) ?
C3 C2 C4 . . 111.3(4) ?
C3 C2 C4 4_565 . 111.3(4) ?
C2 C3 H3A . . 109.5 ?
C2 C3 H3B . . 109.5 ?
H3A C3 H3B . . 109.5 ?
C2 C3 H3C . . 109.5 ?
H3A C3 H3C . . 109.5 ?
H3B C3 H3C . . 109.5 ?
C2 C4 H4A . . 109.5 ?
C2 C4 H4B . . 109.5 ?
H4A C4 H4B . . 109.5 ?
C2 C4 H4C . . 109.5 ?
H4A C4 H4C . . 109.5 ?
H4B C4 H4C . . 109.5 ?
C1 N1 Sb1 . . 176.7(6) ?
F3 Sb1 F4 . . 90.05(11) ?
F3 Sb1 F4 . 4_565 90.05(11) ?
F4 Sb1 F4 . 4_565 175.96(19) ?
F3 Sb1 F1 . . 92.9(2) ?
F4 Sb1 F1 . . 92.01(9) ?
F4 Sb1 F1 4_565 . 92.01(9) ?
F3 Sb1 F2 . . 173.8(2) ?
F4 Sb1 F2 . . 89.73(11) ?
F4 Sb1 F2 4_565 . 89.73(11) ?
F1 Sb1 F2 . . 93.4(2) ?
F3 Sb1 N1 . . 86.6(2) ?
F4 Sb1 N1 . . 87.99(9) ?
F4 Sb1 N1 4_565 . 87.99(9) ?
F1 Sb1 N1 . . 179.4(3) ?
F2 Sb1 N1 . . 87.2(2) ?

_shelx_res_file                  
;


    twin_0t.res created by SHELXL-2014/7


TITL twin_0t.res in P2(1)/m
CELL  0.71073   5.9704   8.8971   9.2014   90.000   97.380   90.000
ZERR    1.000   0.0030   0.0045   0.0046    0.000    0.008    0.000
LATT 1
SYMM -X, 1/2+Y, -Z
SFAC C  H  F  N  Sb
UNIT 10 18 10 2 2
LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
REM Old TITL twin_0m in P2(1)
REM SHELXT solution in P2(1)/m
REM R1 0.088,  Rweak 0.012,  Alpha 0.037,  Orientation as input
REM Formula found by SHELXT:  C10 N Sb
L.S. 10
BOND $H
ACTA 55
CONF
FMAP 2
PLAN 20
TEMP -173.160
WGHT    0.018600    2.726800
BASF   0.23832
FVAR       0.68582
C1    1    0.789677    0.250000    0.631620    10.50000    0.01812    0.01801 =
         0.01957    0.00000    0.00446    0.00000
C2    1    0.932413    0.250000    0.774406    10.50000    0.01807    0.02583 =
         0.01554    0.00000   -0.00251    0.00000
C3    1    1.079708    0.391884    0.783594    11.00000    0.02350    0.02591 =
         0.03057    0.00006   -0.00332   -0.00387
AFIX 137
H3A   2    1.173356    0.391417    0.703581    11.00000   -1.50000
H3B   2    1.177150    0.393722    0.877789    11.00000   -1.50000
H3C   2    0.982683    0.481122    0.775278    11.00000   -1.50000
AFIX   0
C4    1    0.772245    0.250000    0.894074    10.50000    0.02350    0.04035 =
         0.02154    0.00000    0.00297    0.00000
AFIX 137
H4A   2    0.657263    0.328182    0.872074    10.50000   -1.50000
H4B   2    0.859473    0.270104    0.989747    10.50000   -1.50000
H4C   2    0.698624    0.151714    0.896143    10.50000   -1.50000
AFIX   0
F1    3    0.253013    0.250000    0.149993    10.50000    0.03347    0.04230 =
         0.02253    0.00000   -0.01274    0.00000
F2    3    0.215892    0.250000    0.441880    10.50000    0.02219    0.04468 =
         0.02592    0.00000    0.00566    0.00000
F3    3    0.706006    0.250000    0.227864    10.50000    0.02983    0.03987 =
         0.02062    0.00000    0.01132    0.00000
F4    3    0.456887    0.459745    0.331634    11.00000    0.03570    0.01734 =
         0.03106    0.00150   -0.00272    0.00306
N1    4    0.675451    0.250000    0.520951    10.50000    0.01782    0.02122 =
         0.01552    0.00000   -0.00270    0.00000
SB1   5    0.450594    0.250000    0.325213    10.50000    0.01856    0.01707 =
         0.01429    0.00000    0.00030    0.00000
HKLF 5

REM  twin_0t.res in P2(1)/m
REM R1 =  0.0398 for    1334 Fo > 4sig(Fo)  and  0.0649 for all    1532 data
REM     70 parameters refined using      0 restraints

END

WGHT      0.0186      2.7268

REM Highest difference peak  1.292,  deepest hole -2.683,  1-sigma level  0.256
Q1    1   0.3569  0.2500  0.2033  10.50000  0.05    1.29
Q2    1   0.6392  0.2027  0.2965  11.00000  0.05    1.29
Q3    1   0.5211  0.1919  0.3241  11.00000  0.05    1.23
Q4    1   0.2846  0.2500  0.3840  10.50000  0.05    1.22
Q5    1   0.7761  0.2500  0.2977  10.50000  0.05    1.17
Q6    1   0.3748  0.1913  0.3189  11.00000  0.05    1.06
Q7    1   0.8450  0.2500  0.1822  10.50000  0.05    1.06
Q8    1   1.0422  0.6398  0.6781  11.00000  0.05    1.06
Q9    1   0.8628  0.1873  0.2585  11.00000  0.05    1.03
Q10   1   0.5783  0.2016  0.4371  11.00000  0.05    1.01
Q11   1   0.3822  0.2084  0.4577  11.00000  0.05    1.01
Q12   1   0.9868  0.2500  1.0632  10.50000  0.05    0.99
Q13   1   0.3787  0.2500  0.1000  10.50000  0.05    0.98
Q14   1   0.1170  0.1999  0.2416  11.00000  0.05    0.98
Q15   1   0.5772  0.2500  0.1238  10.50000  0.05    0.96
Q16   1   0.1158  0.2500  0.3326  10.50000  0.05    0.93
Q17   1   0.4711  0.2001  0.1861  11.00000  0.05    0.88
Q18   1   0.5093  0.2500  0.5451  10.50000  0.05    0.84
Q19   1   0.8852  0.3643  1.0322  11.00000  0.05    0.82
Q20   1   0.0000  0.2500  0.1817  10.50000  0.05    0.80
;
_shelx_res_checksum              56137
####################################################################### 
# 
# 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_I_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1855716'
_audit_update_record             
;
2018-07-13 deposited with the CCDC.
2018-11-14 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C3 H2 As2 F10 N2'
_chemical_formula_sum            'C3 H2 As2 F10 N2'
_chemical_formula_iupac          ?
_chemical_formula_weight         405.91
_chemical_absolute_configuration ?

_chemical_melting_point          ?

_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
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                   7.5930(13)
_cell_length_b                   10.1881(18)
_cell_length_c                   12.803(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     990.4(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9931
_cell_measurement_theta_min      2.5549
_cell_measurement_theta_max      30.4471
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       rod
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_crystal_density_diffrn    2.722
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             760

_exptl_absorpt_coefficient_mu    6.878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5 (Bruker AXS, 2014)'
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_T_max  0.72

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'fine-focus tube'
_diffrn_source_type              ?

_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'

_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega- and phi-scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            24363
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_theta_min         2.56
_diffrn_reflns_theta_max         30.47
_diffrn_reflns_theta_full        30.47
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18

_refine_special_details          
'Refined as a 2-component perfect inversion twin.'

_reflns_number_total             3002
_reflns_number_gt                2758
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0207
_refine_ls_wR_factor_gt          0.0375
_refine_ls_wR_factor_ref         0.0387
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_refine_ls_number_reflns         3002
_refine_ls_number_parameters     154
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0121P)²+0.4306P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.374
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Refined as a perfect inversion twin.'
_refine_ls_abs_structure_Flack   0.500000

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'
N N 0.0061 0.0033 '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'

_computing_data_collection       
'Bruker Instrument Service v2012.12.0.3 (Bruker AXS, 2012)'
_computing_cell_refinement       'APEX2 v2014.11-0 (Bruker AXS, 2014)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS, 2013)'
_computing_structure_solution    'SHELXTL XT 2014/4 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXTL XL 2014/7 (Bruker AXS, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXTL XT 2014/4 (Bruker AXS, 2014)'

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
As As1 0.49615(5) 0.94566(3) 0.42531(2) 0.01171(7) Uani d . . . 1 . .
As As2 0.48030(4) 0.25857(3) 0.71591(2) 0.01241(7) Uani d . . . 1 . .
C C1 0.4832(5) 0.6355(3) 0.4144(2) 0.0133(5) Uani d . . . 1 . .
C C2 0.4807(5) 0.4917(3) 0.4019(2) 0.0123(6) Uani d . . . 1 . .
H H2A 0.5857 0.4638 0.3618 0.015 Uiso calc U . R 1 . .
H H2B 0.3747 0.4658 0.3619 0.015 Uiso calc U . R 1 . .
C C3 0.4797(4) 0.4244(3) 0.5041(2) 0.0141(6) Uani d . . . 1 . .
F F1 0.6789(3) 0.9286(2) 0.3500(2) 0.0325(6) Uani d . . . 1 . .
F F2 0.3704(3) 0.9412(3) 0.31597(15) 0.0267(5) Uani d . . . 1 . .
F F3 0.3103(3) 0.9348(2) 0.49952(16) 0.0232(5) Uani d . . . 1 . .
F F4 0.6214(3) 0.9253(2) 0.53379(17) 0.0279(5) Uani d . . . 1 . .
F F5 0.5057(3) 1.11110(16) 0.42942(14) 0.0237(4) Uani d . . . 1 . .
F F6 0.6547(3) 0.1798(2) 0.65968(19) 0.0263(6) Uani d . . . 1 . .
F F7 0.3415(3) 0.1589(2) 0.64771(18) 0.0234(5) Uani d . . . 1 . .
F F8 0.3045(3) 0.3509(2) 0.75242(15) 0.0253(5) Uani d . . . 1 . .
F F9 0.6199(3) 0.3736(2) 0.76351(17) 0.0279(5) Uani d . . . 1 . .
F F10 0.4802(3) 0.16684(17) 0.82540(13) 0.0214(4) Uani d . . . 1 . .
N N1 0.4852(3) 0.7455(2) 0.42028(17) 0.0149(4) Uani d . . . 1 . .
N N2 0.4795(4) 0.3691(2) 0.58044(19) 0.0166(5) Uani d . . . 1 . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
As1 0.00930(13) 0.01259(12) 0.01323(12) -0.00001(16) 0.00137(15) 0.00086(11)
As2 0.01244(13) 0.01140(13) 0.01339(13) 0.00070(14) 0.00062(13) 0.00153(11)
C1 0.0078(14) 0.0216(14) 0.0105(12) -0.0019(14) -0.0017(13) 0.0008(11)
C2 0.0130(15) 0.0125(12) 0.0113(12) 0.0006(13) 0.0002(12) -0.0004(10)
C3 0.0123(14) 0.0111(12) 0.0191(14) 0.0001(13) 0.0017(13) -0.0036(11)
F1 0.0221(11) 0.0227(12) 0.0526(15) -0.0041(10) 0.0246(11) -0.0023(12)
F2 0.0361(12) 0.0259(12) 0.0180(11) 0.0022(11) -0.0094(9) 0.0031(10)
F3 0.0167(10) 0.0260(12) 0.0268(11) -0.0002(9) 0.0118(8) -0.0020(10)
F4 0.0286(11) 0.0224(12) 0.0325(13) -0.0019(10) -0.0189(10) -0.0006(10)
F5 0.0295(10) 0.0130(8) 0.0288(10) -0.0001(10) 0.0044(13) -0.0003(7)
F6 0.0217(11) 0.0309(14) 0.0264(13) 0.0142(10) 0.0059(10) 0.0047(11)
F7 0.0286(12) 0.0223(12) 0.0193(11) -0.0107(9) -0.0022(9) 0.0006(10)
F8 0.0279(12) 0.0280(13) 0.0199(12) 0.0142(10) 0.0080(9) 0.0052(10)
F9 0.0325(13) 0.0277(13) 0.0235(12) -0.0158(10) -0.0040(10) -0.0021(10)
F10 0.0231(11) 0.0223(9) 0.0190(9) 0.0007(10) -0.0015(9) 0.0084(7)
N1 0.0116(10) 0.0171(11) 0.0159(11) -0.0009(14) -0.0016(11) 0.0038(11)
N2 0.0176(14) 0.0140(11) 0.0181(12) 0.0008(11) 0.0021(13) -0.0018(10)

_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
As1 F5 . 1.6879(17) ?
As1 F2 . 1.695(2) ?
As1 F4 . 1.696(2) ?
As1 F1 . 1.698(2) ?
As1 F3 . 1.7049(19) ?
As1 N1 . 2.042(3) ?
As2 F10 . 1.6848(17) ?
As2 F9 . 1.694(2) ?
As2 F8 . 1.698(2) ?
As2 F7 . 1.704(2) ?
As2 F6 . 1.707(2) ?
As2 N2 . 2.068(3) ?
C1 N1 . 1.123(4) ?
C1 C2 . 1.474(4) ?
C2 C3 . 1.476(4) ?
C2 H2A . 0.99 ?
C2 H2B . 0.99 ?
C3 N2 . 1.129(4) ?

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
F5 As1 F2 . . 94.41(11) ?
F5 As1 F4 . . 94.17(11) ?
F2 As1 F4 . . 171.42(13) ?
F5 As1 F1 . . 94.87(12) ?
F2 As1 F1 . . 89.34(12) ?
F4 As1 F1 . . 89.68(12) ?
F5 As1 F3 . . 94.76(12) ?
F2 As1 F3 . . 89.56(11) ?
F4 As1 F3 . . 89.98(12) ?
F1 As1 F3 . . 170.37(13) ?
F5 As1 N1 . . 179.86(11) ?
F2 As1 N1 . . 85.65(11) ?
F4 As1 N1 . . 85.77(10) ?
F1 As1 N1 . . 85.01(11) ?
F3 As1 N1 . . 85.36(10) ?
F10 As2 F9 . . 94.86(10) ?
F10 As2 F8 . . 94.46(10) ?
F9 As2 F8 . . 90.54(12) ?
F10 As2 F7 . . 95.47(11) ?
F9 As2 F7 . . 169.65(11) ?
F8 As2 F7 . . 89.16(11) ?
F10 As2 F6 . . 95.20(11) ?
F9 As2 F6 . . 89.51(12) ?
F8 As2 F6 . . 170.30(10) ?
F7 As2 F6 . . 89.05(10) ?
F10 As2 N2 . . 179.28(9) ?
F9 As2 N2 . . 85.80(11) ?
F8 As2 N2 . . 85.82(10) ?
F7 As2 N2 . . 83.86(11) ?
F6 As2 N2 . . 84.51(11) ?
N1 C1 C2 . . 177.7(3) ?
C1 C2 C3 . . 111.5(2) ?
C1 C2 H2A . . 109.3 ?
C3 C2 H2A . . 109.3 ?
C1 C2 H2B . . 109.3 ?
C3 C2 H2B . . 109.3 ?
H2A C2 H2B . . 108.0 ?
N2 C3 C2 . . 177.7(3) ?
C1 N1 As1 . . 177.4(2) ?
C3 N2 As2 . . 177.0(2) ?

_shelx_res_file                  
;
TITL final_b.res in P2(1)2(1)2(1)
CELL  0.71073   7.5930  10.1881  12.8034   90.000   90.000   90.000
ZERR    4.000   0.0013   0.0018   0.0023    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  N  F  As
UNIT 12 8 8 40 8
LIST 4
L.S. 10
ACTA 58
CONF
BOND $H
FMAP 2
PLAN 4
SIZE 0.050 0.050 0.180
TWIN
TEMP -173.140
WGHT    0.012100    0.430600
FVAR       0.32144
AS1   5    0.496147    0.945659    0.425312    11.00000    0.00930    0.01259 =
         0.01323    0.00086    0.00137   -0.00001
AS2   5    0.480297    0.258571    0.715909    11.00000    0.01244    0.01140 =
         0.01339    0.00153    0.00062    0.00070
C1    1    0.483250    0.635483    0.414378    11.00000    0.00778    0.02158 =
         0.01050    0.00083   -0.00171   -0.00192
C2    1    0.480719    0.491705    0.401943    11.00000    0.01305    0.01248 =
         0.01133   -0.00042    0.00016    0.00059
AFIX  23
H2A   2    0.585656    0.463801    0.361781    11.00000   -1.20000
H2B   2    0.374742    0.465850    0.361874    11.00000   -1.20000
AFIX   0
C3    1    0.479671    0.424443    0.504063    11.00000    0.01232    0.01106 =
         0.01905   -0.00359    0.00169    0.00012
F1    4    0.678864    0.928583    0.350005    11.00000    0.02207    0.02273 =
         0.05257   -0.00229    0.02461   -0.00407
F2    4    0.370402    0.941174    0.315974    11.00000    0.03607    0.02594 =
         0.01800    0.00308   -0.00941    0.00219
F3    4    0.310280    0.934808    0.499522    11.00000    0.01668    0.02597 =
         0.02682   -0.00195    0.01176   -0.00017
F4    4    0.621351    0.925265    0.533795    11.00000    0.02865    0.02244 =
         0.03251   -0.00058   -0.01890   -0.00193
F5    4    0.505714    1.111101    0.429419    11.00000    0.02946    0.01297 =
         0.02878   -0.00032    0.00439   -0.00009
F6    4    0.654698    0.179833    0.659681    11.00000    0.02172    0.03089 =
         0.02639    0.00466    0.00593    0.01422
F7    4    0.341547    0.158856    0.647707    11.00000    0.02859    0.02233 =
         0.01933    0.00056   -0.00224   -0.01067
F8    4    0.304530    0.350899    0.752423    11.00000    0.02786    0.02797 =
         0.01994    0.00518    0.00798    0.01422
F9    4    0.619881    0.373595    0.763506    11.00000    0.03251    0.02768 =
         0.02349   -0.00206   -0.00397   -0.01579
F10   4    0.480172    0.166842    0.825404    11.00000    0.02309    0.02227 =
         0.01896    0.00836   -0.00146    0.00073
N1    3    0.485215    0.745454    0.420281    11.00000    0.01164    0.01712 =
         0.01586    0.00376   -0.00157   -0.00095
N2    3    0.479522    0.369097    0.580438    11.00000    0.01761    0.01400 =
         0.01810   -0.00177    0.00214    0.00083
HKLF 4

REM  final_b.res in P2(1)2(1)2(1)
REM R1 =  0.0207 for    2758 Fo > 4sig(Fo)  and  0.0258 for all    3002 data
REM    154 parameters refined using      0 restraints

END

WGHT      0.0121      0.4306

REM Highest difference peak  0.341,  deepest hole -0.374,  1-sigma level  0.081
Q1    1   0.4325  0.2046  0.7802  11.00000  0.05    0.34
Q2    1   0.4407  0.1845  0.6549  11.00000  0.05    0.33
Q3    1   0.5222  0.1770  0.6601  11.00000  0.05    0.31
Q4    1   0.4884  0.2406  0.7882  11.00000  0.05    0.30
;
_shelx_res_checksum              78551
####################################################################### 
# 
# 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_PhCNAsF5
_database_code_depnum_ccdc_archive 'CCDC 1855717'
_audit_update_record             
;
2018-07-13 deposited with the CCDC.
2018-11-14 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            PhCNAsF5
_chemical_formula_moiety         'C7 H5 As F5 N'
_chemical_formula_sum            'C7 H5 As F5 N'
_chemical_formula_iupac          ?
_chemical_formula_weight         273.04

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   11.705(5)
_cell_length_b                   12.542(6)
_cell_length_c                   8.136(4)
_cell_angle_alpha                90
_cell_angle_beta                 131.518(7)
_cell_angle_gamma                90
_cell_volume                     894.3(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3795
_cell_measurement_theta_min      2.8340
_cell_measurement_theta_max      29.3431
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_exptl_crystal_density_diffrn    2.028
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             528

_exptl_absorpt_coefficient_mu    3.838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5 (Bruker AXS, 2014)'
_exptl_absorpt_correction_T_min  0.479
_exptl_absorpt_correction_T_max  0.746

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'fine-focus tube'
_diffrn_source_type              ?

_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'

_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega- and phi-scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            9247
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_theta_min         2.83
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_full        28.27
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10

_refine_special_details          
;
;

_reflns_number_total             1120
_reflns_number_gt                1025
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0341
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0914
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.072
_refine_ls_number_reflns         1120
_refine_ls_number_parameters     67
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0641P)²+0.2125P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         2.122
_refine_diff_density_min         -1.174
_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'
N N 0.0061 0.0033 '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'

_computing_data_collection       
'Bruker Instrument Service v2012.12.0.3 (Bruker AXS, 2012)'
_computing_cell_refinement       'APEX3 v2016.1-0 (Bruker AXS, 2016)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS, 2013)'
_computing_structure_solution    'SHELXTL XT 2014/5 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXTL XL 2014/7 (Bruker AXS, 2014)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 758)'
_computing_publication_material  'SHELXTL XL 2014/7 (Bruker AXS, 2014)'

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
C C1 0.5 0.3788(3) 0.25 0.0242(7) Uani d T P S 1 . .
C C2 0.5 0.4929(3) 0.25 0.0217(7) Uani d T P S 1 . .
C C3 0.6129(3) 0.5478(2) 0.4477(4) 0.0223(5) Uani d . . . 1 . .
H H3 0.6882 0.5097 0.5797 0.027 Uiso calc U . R 1 . .
C C4 0.6116(3) 0.6578(2) 0.4455(4) 0.0245(5) Uani d . . . 1 . .
H H4 0.6868 0.696 0.5772 0.029 Uiso calc U . R 1 . .
C C5 0.5 0.7135(3) 0.25 0.0238(7) Uani d T P S 1 . .
H H5 0.5 0.7892 0.25 0.029 Uiso calc U P R 1 . .
N N1 0.5 0.2872(2) 0.25 0.0253(6) Uani d T P S 1 . .
F F1 0.5 -0.00684(17) 0.25 0.0315(5) Uani d T P S 1 . .
F F2 0.3734(2) 0.13645(11) 0.2897(3) 0.0321(4) Uani d . . . 1 . .
F F3 0.6493(2) 0.13690(12) 0.5273(3) 0.0344(4) Uani d . . . 1 . .
As As1 0.5 0.12879(2) 0.25 0.02006(16) Uani d T P S 1 . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
C1 0.0253(17) 0.0254(18) 0.0219(17) 0 0.0155(15) 0
C2 0.0262(17) 0.0204(16) 0.0222(16) 0 0.0176(14) 0
C3 0.0218(11) 0.0251(11) 0.0168(11) 0.0026(9) 0.0114(9) 0.0036(9)
C4 0.0237(11) 0.0278(12) 0.0194(11) -0.0024(10) 0.0132(10) -0.0028(10)
C5 0.0274(18) 0.0196(16) 0.0242(18) 0 0.0171(16) 0
N1 0.0262(16) 0.0218(15) 0.0248(16) 0 0.0156(14) 0
F1 0.0380(12) 0.0167(10) 0.0341(12) 0 0.0215(10) 0
F2 0.0353(9) 0.0269(8) 0.0410(11) -0.0056(6) 0.0282(9) -0.0060(6)
F3 0.0311(9) 0.0334(10) 0.0154(8) -0.0031(6) 0.0055(7) 0.0011(6)
As1 0.0204(2) 0.0170(2) 0.0146(2) 0 0.00810(17) 0

_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
C1 N1 . 1.148(4) ?
C1 C2 . 1.432(5) ?
C2 C3 . 1.410(3) ?
C2 C3 2_655 1.410(3) ?
C3 C4 . 1.380(4) ?
C3 H3 . 0.95 ?
C4 C5 . 1.404(3) ?
C4 H4 . 0.95 ?
C5 C4 2_655 1.404(3) ?
C5 H5 . 0.95 ?
N1 As1 . 1.987(3) ?
F1 As1 . 1.701(2) ?
F2 As1 . 1.7157(19) ?
F3 As1 . 1.7108(19) ?
As1 F3 2_655 1.7107(19) ?
As1 F2 2_655 1.7157(19) ?

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
N1 C1 C2 . . 180.0 ?
C3 C2 C3 . 2_655 121.6(3) ?
C3 C2 C1 . . 119.19(16) ?
C3 C2 C1 2_655 . 119.19(16) ?
C4 C3 C2 . . 118.6(2) ?
C4 C3 H3 . . 120.7 ?
C2 C3 H3 . . 120.7 ?
C3 C4 C5 . . 120.4(2) ?
C3 C4 H4 . . 119.8 ?
C5 C4 H4 . . 119.8 ?
C4 C5 C4 . 2_655 120.3(3) ?
C4 C5 H5 . . 119.9 ?
C4 C5 H5 2_655 . 119.9 ?
C1 N1 As1 . . 180.0 ?
F1 As1 F3 . 2_655 93.41(5) ?
F1 As1 F3 . . 93.41(5) ?
F3 As1 F3 2_655 . 173.18(10) ?
F1 As1 F2 . 2_655 93.21(5) ?
F3 As1 F2 2_655 2_655 90.18(10) ?
F3 As1 F2 . 2_655 89.43(10) ?
F1 As1 F2 . . 93.21(5) ?
F3 As1 F2 2_655 . 89.43(10) ?
F3 As1 F2 . . 90.18(10) ?
F2 As1 F2 2_655 . 173.58(10) ?
F1 As1 N1 . . 180.0 ?
F3 As1 N1 2_655 . 86.59(5) ?
F3 As1 N1 . . 86.59(5) ?
F2 As1 N1 2_655 . 86.79(5) ?
F2 As1 N1 . . 86.79(5) ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C3 C2 C3 C4 2_655 . . . 0.00(15) ?
C1 C2 C3 C4 . . . . 180.00(15) ?
C2 C3 C4 C5 . . . . 0.0(3) ?
C3 C4 C5 C4 . . . 2_655 0.00(16) ?

_shelx_res_file                  
;


    final.res created by SHELXL-2014/7


CELL  0.71073  11.7051  12.5423   8.1358   90.000  131.518   90.000
ZERR    4.000   0.0053   0.0055   0.0036    0.000    0.007    0.000
LATT  7
SYMM -X, Y, 1/2-Z
SFAC C H N F AS
UNIT 28 20 4 20 4
TEMP -173.150
L.S. 10
SHEL 999 0.75
ACTA 55
BOND $H
CONF
LIST 4
FMAP 2
PLAN 4
WGHT    0.064100    0.212500
FVAR       0.11638
C1    1    0.500000    0.378758    0.250000    10.50000    0.02528    0.02542 =
         0.02185    0.00000    0.01554    0.00000
C2    1    0.500000    0.492903    0.250000    10.50000    0.02619    0.02037 =
         0.02223    0.00000    0.01758    0.00000
C3    1    0.612896    0.547751    0.447741    11.00000    0.02179    0.02509 =
         0.01677    0.00362    0.01145    0.00256
AFIX  43
H3    2    0.688246    0.509747    0.579714    11.00000   -1.20000
AFIX   0
C4    1    0.611617    0.657758    0.445507    11.00000    0.02369    0.02779 =
         0.01938   -0.00281    0.01322   -0.00236
AFIX  43
H4    2    0.686771    0.696044    0.577152    11.00000   -1.20000
AFIX   0
C5    1    0.500000    0.713467    0.250000    10.50000    0.02745    0.01961 =
         0.02419    0.00000    0.01706    0.00000
AFIX  43
H5    2    0.500001    0.789210    0.250002    10.50000   -1.20000
AFIX   0
N1    3    0.500000    0.287207    0.250000    10.50000    0.02617    0.02181 =
         0.02475    0.00000    0.01560    0.00000
F1    4    0.500000   -0.006838    0.250000    10.50000    0.03799    0.01671 =
         0.03414    0.00000    0.02147    0.00000
F2    4    0.373398    0.136455    0.289674    11.00000    0.03532    0.02691 =
         0.04103   -0.00598    0.02823   -0.00563
F3    4    0.649278    0.136905    0.527269    11.00000    0.03110    0.03343 =
         0.01538    0.00106    0.00554   -0.00311
AS1   5    0.500000    0.128792    0.250000    10.50000    0.02038    0.01702 =
         0.01456    0.00000    0.00810    0.00000
HKLF 4

REM
REM R1 =  0.0341 for    1025 Fo > 4sig(Fo)  and  0.0378 for all    1120 data
REM     67 parameters refined using      0 restraints

END

WGHT      0.0641      0.2125

REM Highest difference peak  2.122,  deepest hole -1.174,  1-sigma level  0.132
Q1    1   0.4231  0.1285  0.2354  11.00000  0.05    2.12
Q2    1   0.2800  0.1356  0.2430  11.00000  0.05    0.51
Q3    1   0.5000  0.2326  0.2500  10.50000  0.05    0.41
Q4    1   0.5778  0.1473  0.5040  11.00000  0.05    0.40
;
_shelx_res_checksum              75838
####################################################################### 
# 
# 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_TS408
_database_code_depnum_ccdc_archive 'CCDC 1855719'
_audit_update_record             
;
2018-07-13 deposited with the CCDC.
2018-11-14 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C10 H18 As2 F10 N2'
_chemical_formula_sum            'C10 H18 As2 F10 N2'
_chemical_formula_iupac          ?
_chemical_formula_weight         506.10

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/m 1'
_space_group_name_Hall           '-P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   5.9896(16)
_cell_length_b                   8.660(2)
_cell_length_c                   8.905(2)
_cell_angle_alpha                90
_cell_angle_beta                 97.932(4)
_cell_angle_gamma                90
_cell_volume                     457.5(2)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    57
_cell_measurement_theta_min      3.2279
_cell_measurement_theta_max      23.1985
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.142
_exptl_crystal_density_diffrn    1.837
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             248

_exptl_absorpt_coefficient_mu    3.742
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   'SADABS 2014/5 (Bruker AXS, 2014)'
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5691


_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'fine-focus tube'
_diffrn_source_type              ?

_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'

_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega- and phi-scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            9013
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_theta_min         2.31
_diffrn_reflns_theta_max         30.55
_diffrn_reflns_theta_full        30.55
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12

_refine_special_details          
;
;

_reflns_number_total             1482
_reflns_number_gt                1366
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0217
_refine_ls_R_factor_gt           0.0184
_refine_ls_wR_factor_gt          0.0444
_refine_ls_wR_factor_ref         0.0456
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_refine_ls_number_reflns         1482
_refine_ls_number_parameters     69
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0146P)²+0.0888P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.334
_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'
As As 0.0499 2.0058 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       
'Bruker Instrument Service v2012.12.0.3 (Bruker AXS, 2012)'
_computing_cell_refinement       'APEX3 v2016.9-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS, 2013)'
_computing_structure_solution    'SHELXTL XT 2014/4 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 807)'
_computing_publication_material  'SHELXTL XT 2014/4 (Bruker AXS, 2014)'

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
C C1 0.7784(3) 0.25 0.6220(2) 0.0159(3) Uani d T P S 1 . .
C C2 0.9290(3) 0.25 0.7673(2) 0.0158(3) Uani d T P S 1 . .
C C3 1.0766(2) 0.39603(16) 0.77271(16) 0.0232(3) Uani d . . . 1 . .
H H3A 1.1626 0.3956 0.6867 0.035 Uiso calc U . R 1 . .
H H3B 1.1809 0.3976 0.8677 0.035 Uiso calc U . R 1 . .
H H3C 0.9802 0.4879 0.7672 0.035 Uiso calc U . R 1 . .
C C4 0.7803(3) 0.25 0.8951(2) 0.0240(4) Uani d T P S 1 . .
H H4A 0.6729 0.3358 0.8799 0.036 Uiso calc U P R 0.5 . .
H H4B 0.8756 0.262 0.9931 0.024 Uiso calc U P R 0.5 . .
H H4C 0.6978 0.1522 0.8938 0.036 Uiso calc U P R 0.5 . .
As As1 0.45088(3) 0.25 0.31923(2) 0.01420(6) Uani d T P S 1 . .
F F1 0.23578(19) 0.25 0.42687(13) 0.0281(3) Uani d T P S 1 . .
F F2 0.45877(13) 0.44741(9) 0.32748(9) 0.02626(19) Uani d . . . 1 . .
F F3 0.2711(2) 0.25 0.15329(13) 0.0298(3) Uani d T P S 1 . .
F F4 0.6846(2) 0.25 0.22973(13) 0.0277(3) Uani d T P S 1 . .
N N1 0.6598(3) 0.25 0.51047(17) 0.0173(3) Uani d T P S 1 . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
C1 0.0182(8) 0.0128(7) 0.0173(8) 0 0.0041(6) 0
C2 0.0143(7) 0.0179(8) 0.0140(7) 0 -0.0021(6) 0
C3 0.0209(6) 0.0219(6) 0.0249(7) -0.0048(5) -0.0040(5) -0.0008(5)
C4 0.0223(9) 0.0356(11) 0.0141(8) 0 0.0021(7) 0
As1 0.01636(10) 0.01489(9) 0.01055(9) 0 -0.00101(6) 0
F1 0.0187(5) 0.0422(7) 0.0240(6) 0 0.0051(5) 0
F2 0.0324(5) 0.0154(4) 0.0285(4) 0.0026(3) -0.0048(4) 0.0020(3)
F3 0.0335(7) 0.0343(7) 0.0173(6) 0 -0.0115(5) 0
F4 0.0281(6) 0.0382(7) 0.0186(6) 0 0.0096(5) 0
N1 0.0188(7) 0.0175(7) 0.0145(7) 0 -0.0017(6) 0

_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
C1 N1 . 1.139(2) ?
C1 C2 . 1.471(2) ?
C2 C4 . 1.539(2) ?
C2 C3 . 1.5398(17) ?
C2 C3 4_565 1.5398(17) ?
C3 H3A . 0.98 ?
C3 H3B . 0.98 ?
C3 H3C . 0.98 ?
C4 H4A . 0.98 ?
C4 H4B . 0.98 ?
C4 H4C . 0.98 ?
As1 F4 . 1.7036(12) ?
As1 F3 . 1.7041(11) ?
As1 F1 . 1.7087(12) ?
As1 F2 . 1.7115(9) ?
As1 F2 4_565 1.7115(9) ?
As1 N1 . 1.9692(15) ?

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
N1 C1 C2 . . 179.23(18) ?
C1 C2 C4 . . 107.65(14) ?
C1 C2 C3 . . 107.90(10) ?
C4 C2 C3 . . 111.40(10) ?
C1 C2 C3 . 4_565 107.90(10) ?
C4 C2 C3 . 4_565 111.40(10) ?
C3 C2 C3 . 4_565 110.43(15) ?
C2 C3 H3A . . 109.5 ?
C2 C3 H3B . . 109.5 ?
H3A C3 H3B . . 109.5 ?
C2 C3 H3C . . 109.5 ?
H3A C3 H3C . . 109.5 ?
H3B C3 H3C . . 109.5 ?
C2 C4 H4A . . 109.5 ?
C2 C4 H4B . . 109.5 ?
H4A C4 H4B . . 109.5 ?
C2 C4 H4C . . 109.5 ?
H4A C4 H4C . . 109.5 ?
H4B C4 H4C . . 109.5 ?
F4 As1 F3 . . 93.22(6) ?
F4 As1 F1 . . 173.85(5) ?
F3 As1 F1 . . 92.94(6) ?
F4 As1 F2 . . 90.03(3) ?
F3 As1 F2 . . 92.73(3) ?
F1 As1 F2 . . 89.68(3) ?
F4 As1 F2 . 4_565 90.03(3) ?
F3 As1 F2 . 4_565 92.73(3) ?
F1 As1 F2 . 4_565 89.68(3) ?
F2 As1 F2 . 4_565 174.53(5) ?
F4 As1 N1 . . 86.53(6) ?
F3 As1 N1 . . 179.75(6) ?
F1 As1 N1 . . 87.31(6) ?
F2 As1 N1 . . 87.27(3) ?
F2 As1 N1 4_565 . 87.27(3) ?
C1 N1 As1 . . 179.17(15) ?

_shelx_res_file                  
;


    final_a.res created by SHELXL-2014/7


TITL final_a.res in P2(1)/m
REM Old TITL final in P2(1)
REM SHELXT solution in P2(1)/m
REM R1 0.107,  Rweak 0.007,  Alpha 0.044,  Orientation as input
REM Formula found by SHELXT:  C9 As N2
CELL  0.71073   5.9896   8.6601   8.9051   90.000   97.932   90.000
ZERR    1.000   0.0016   0.0023   0.0024    0.000    0.004    0.000
LATT  1
SYMM -X, 1/2+Y, -Z
SFAC C H AS F N
UNIT 10 18 2 10 2
TEMP -173.140
L.S. 10
BOND $H
LIST 4
ACTA
CONF
FMAP 2
PLAN 20
WGHT    0.014600    0.088800
FVAR       0.91033
C1    1    0.778393    0.250000    0.622025    10.50000    0.01825    0.01276 =
         0.01726    0.00000    0.00406    0.00000
C2    1    0.928994    0.250000    0.767266    10.50000    0.01426    0.01795 =
         0.01399    0.00000   -0.00212    0.00000
C3    1    1.076558    0.396026    0.772712    11.00000    0.02088    0.02193 =
         0.02492   -0.00078   -0.00399   -0.00484
AFIX 137
H3A   2    1.162556    0.395563    0.686734    11.00000   -1.50000
H3B   2    1.180866    0.397592    0.867718    11.00000   -1.50000
H3C   2    0.980170    0.487863    0.767151    11.00000   -1.50000
AFIX   0
C4    1    0.780313    0.250000    0.895113    10.50000    0.02226    0.03563 =
         0.01414    0.00000    0.00213    0.00000
AFIX 137
H4A   2    0.672907    0.335809    0.879874    10.50000   -1.50000
H4B   2    0.875587    0.262002    0.993098    10.50000   -1.00000
H4C   2    0.697777    0.152189    0.893767    10.50000   -1.50000
AFIX   0
AS1   3    0.450876    0.250000    0.319226    10.50000    0.01636    0.01489 =
         0.01055    0.00000   -0.00101    0.00000
F1    4    0.235777    0.250000    0.426867    10.50000    0.01873    0.04223 =
         0.02404    0.00000    0.00512    0.00000
F2    4    0.458768    0.447410    0.327480    11.00000    0.03236    0.01541 =
         0.02848    0.00199   -0.00478    0.00262
F3    4    0.271079    0.250000    0.153293    10.50000    0.03352    0.03429 =
         0.01731    0.00000   -0.01149    0.00000
F4    4    0.684574    0.250000    0.229735    10.50000    0.02806    0.03819 =
         0.01862    0.00000    0.00963    0.00000
N1    5    0.659773    0.250000    0.510471    10.50000    0.01875    0.01752 =
         0.01451    0.00000   -0.00169    0.00000
HKLF 4

REM  final_a.res in P2(1)/m
REM R1 =  0.0184 for    1366 Fo > 4sig(Fo)  and  0.0217 for all    1482 data
REM     69 parameters refined using      0 restraints

END

WGHT      0.0143      0.0821

REM Highest difference peak  0.343,  deepest hole -0.334,  1-sigma level  0.068
Q1    1   0.6086  0.2500  0.2776  10.50000  0.05    0.34
Q2    1   0.3062  0.2500  0.3774  10.50000  0.05    0.32
Q3    1   1.0063  0.1855  0.7734  11.00000  0.05    0.32
Q4    1   0.3591  0.4284  0.3643  11.00000  0.05    0.27
Q5    1   0.4419  0.4052  0.2751  11.00000  0.05    0.26
Q6    1   0.6552  0.4451  0.3557  11.00000  0.05    0.23
Q7    1   0.1553  0.2500  0.3787  10.50000  0.05    0.23
Q8    1   0.2996  0.4320  0.3009  11.00000  0.05    0.22
Q9    1   0.6589  0.1807  0.1972  11.00000  0.05    0.22
Q10   1   0.6472  0.2500  0.5975  10.50000  0.05    0.21
Q11   1   0.4975  0.4545  0.8252  11.00000  0.05    0.20
Q12   1   0.4327  0.5709  0.3827  11.00000  0.05    0.20
Q13   1   0.8704  0.2500  0.7136  10.50000  0.05    0.20
Q14   1   0.2509  0.1920  0.4619  11.00000  0.05    0.20
Q15   1   0.2230  0.2500  0.3015  10.50000  0.05    0.20
Q16   1   0.0632  0.2500  0.1333  10.50000  0.05    0.20
Q17   1   0.2121  0.2500  0.1767  10.50000  0.05    0.19
Q18   1   1.0571  0.4842  0.9799  11.00000  0.05    0.18
Q19   1   0.8503  0.2299  0.8259  11.00000  0.05    0.18
Q20   1   0.9088  0.2500  0.3613  10.50000  0.05    0.18
;
_shelx_res_checksum              67753
####################################################################### 
# 
# 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_I_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1855721'
_audit_update_record             
;
2018-07-13 deposited with the CCDC.
2018-11-14 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C3 H2 F5 N2 Sb'
_chemical_formula_iupac          ?
_chemical_formula_weight         282.82

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   5.3862(16)
_cell_length_b                   15.562(5)
_cell_length_c                   8.490(3)
_cell_angle_alpha                90
_cell_angle_beta                 102.140(5)
_cell_angle_gamma                90
_cell_volume                     695.7(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8451
_cell_measurement_theta_min      2.6176
_cell_measurement_theta_max      30.4563
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.323
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.078
_exptl_crystal_density_diffrn    2.700
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             520

_exptl_absorpt_coefficient_mu    3.997
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5 (Bruker AXS, 2014)'
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_T_max  0.75

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'fine-focus tube'
_diffrn_source_type              ?

_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'

_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega- and phi-scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            15914
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_theta_min         2.62
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_full        30.50
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12

_refine_special_details          
;
;

_reflns_number_total             2112
_reflns_number_gt                1691
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0402
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1024
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_restrained_S_all      1.107
_refine_ls_number_reflns         2112
_refine_ls_number_parameters     100
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0474P)²+3.0277P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.820
_refine_diff_density_min         -1.064
_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'
N N 0.0061 0.0033 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       
'Bruker Instrument Service v2012.12.0.3 (Bruker AXS, 2012)'
_computing_cell_refinement       'APEX2 v2014.11-0 (Bruker AXS, 2014)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS, 2013)'
_computing_structure_solution    'SHELXTL XT 2014/4 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXTL XL 2014/7 (Bruker AXS, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXTL XT 2014/4 (Bruker AXS, 2014)'

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
C C1 0.6140(10) 0.8332(3) 0.3000(6) 0.0155(9) Uani d . . . 1 . .
C C2 0.7113(10) 0.9208(3) 0.2941(7) 0.0176(10) Uani d . . . 1 . .
H H2A 0.6213 0.9596 0.3558 0.021 Uiso calc U . R 1 . .
H H2B 0.6763 0.9409 0.1809 0.021 Uiso calc U . R 1 . .
C C3 0.9853(10) 0.9255(3) 0.3608(6) 0.0162(9) Uani d . . . 1 . .
F F1 0.2211(7) 0.5449(2) 0.4048(4) 0.0249(7) Uani d . . . 1 . .
F F2 0.2121(7) 0.6432(2) 0.1359(4) 0.0254(7) Uani d . . . 1 . .
F F3 0.1022(7) 0.7141(2) 0.3974(5) 0.0299(8) Uani d . . . 1 . .
F F4 0.5400(8) 0.6629(2) 0.5667(4) 0.0327(9) Uani d . . . 1 . .
F F5 0.6510(6) 0.5932(2) 0.3075(5) 0.0272(7) Uani d . . . 1 . .
N N1 0.5327(8) 0.7657(3) 0.3035(5) 0.0169(8) Uani d . . . 1 . .
N N2 1.1986(9) 0.9325(3) 0.4141(6) 0.0203(9) Uani d . . . 1 . .
Sb Sb1 0.36676(6) 0.64759(2) 0.35362(4) 0.01500(11) Uani d . . . 1 . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
C1 0.015(2) 0.015(2) 0.016(2) 0.0021(17) 0.0018(18) 0.0008(17)
C2 0.019(2) 0.014(2) 0.020(2) -0.0011(18) 0.0044(19) 0.0026(18)
C3 0.020(2) 0.010(2) 0.021(2) 0.0001(18) 0.0102(19) -0.0021(17)
F1 0.0302(18) 0.0163(15) 0.0285(17) -0.0091(13) 0.0069(14) -0.0001(13)
F2 0.0321(18) 0.0217(16) 0.0179(15) -0.0029(14) -0.0047(13) -0.0021(12)
F3 0.0275(18) 0.0197(16) 0.048(2) -0.0024(14) 0.0206(17) -0.0088(15)
F4 0.054(3) 0.0246(18) 0.0145(15) -0.0137(16) -0.0037(16) 0.0009(13)
F5 0.0202(16) 0.0156(15) 0.047(2) 0.0038(13) 0.0101(15) -0.0021(14)
N1 0.019(2) 0.0149(19) 0.0172(19) 0.0008(16) 0.0038(16) 0.0011(15)
N2 0.020(2) 0.017(2) 0.023(2) 0.0000(17) 0.0047(18) -0.0016(17)
Sb1 0.01866(17) 0.01123(16) 0.01497(17) -0.00226(13) 0.00319(11) -0.00078(12)

_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
C1 N1 . 1.141(7) ?
C1 C2 . 1.465(7) ?
C2 C3 . 1.467(8) ?
C2 H2A . 0.99 ?
C2 H2B . 0.99 ?
C3 N2 . 1.148(7) ?
F1 Sb1 . 1.871(3) ?
F2 Sb1 . 1.862(3) ?
F3 Sb1 . 1.860(3) ?
F4 Sb1 . 1.868(3) ?
F5 Sb1 . 1.862(3) ?
N1 Sb1 . 2.126(4) ?

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
N1 C1 C2 . . 178.4(5) ?
C1 C2 C3 . . 111.7(4) ?
C1 C2 H2A . . 109.3 ?
C3 C2 H2A . . 109.3 ?
C1 C2 H2B . . 109.3 ?
C3 C2 H2B . . 109.3 ?
H2A C2 H2B . . 107.9 ?
N2 C3 C2 . . 177.3(5) ?
C1 N1 Sb1 . . 168.9(4) ?
F3 Sb1 F2 . . 90.97(17) ?
F3 Sb1 F5 . . 173.28(15) ?
F2 Sb1 F5 . . 89.46(17) ?
F3 Sb1 F4 . . 89.03(19) ?
F2 Sb1 F4 . . 173.69(15) ?
F5 Sb1 F4 . . 89.80(18) ?
F3 Sb1 F1 . . 92.99(15) ?
F2 Sb1 F1 . . 94.44(15) ?
F5 Sb1 F1 . . 93.66(15) ?
F4 Sb1 F1 . . 91.86(15) ?
F3 Sb1 N1 . . 86.05(16) ?
F2 Sb1 N1 . . 87.26(16) ?
F5 Sb1 N1 . . 87.28(16) ?
F4 Sb1 N1 . . 86.44(16) ?
F1 Sb1 N1 . . 178.06(16) ?

_shelx_res_file                  
;
TITL final_a.res in P2(1)/n
CELL  0.71073   5.3862  15.5624   8.4897   90.000  102.140   90.000
ZERR    4.000   0.0016   0.0045   0.0025    0.000    0.005    0.000
LATT 1
SYMM 1/2-X, 1/2+Y, 1/2-Z
SFAC C  H  N  F  Sb
UNIT 12 8 8 20 4
LIST 4
L.S. 10
ACTA 58
CONF
BOND $H
FMAP 2
PLAN 5
SIZE 0.078 0.171 0.323
TEMP -173.150
WGHT    0.047400    3.027700
FVAR       0.40143
C1    1    0.614000    0.833222    0.299970    11.00000    0.01512    0.01489 =
         0.01585    0.00083    0.00175    0.00214
C2    1    0.711278    0.920833    0.294063    11.00000    0.01930    0.01371 =
         0.01984    0.00258    0.00443   -0.00114
AFIX  23
H2A   2    0.621311    0.959568    0.355835    11.00000   -1.20000
H2B   2    0.676336    0.940877    0.180871    11.00000   -1.20000
AFIX   0
C3    1    0.985279    0.925461    0.360843    11.00000    0.02019    0.01039 =
         0.02072   -0.00211    0.01019    0.00013
F1    4    0.221068    0.544907    0.404821    11.00000    0.03021    0.01627 =
         0.02848   -0.00012    0.00690   -0.00906
F2    4    0.212086    0.643219    0.135911    11.00000    0.03212    0.02172 =
         0.01791   -0.00208   -0.00473   -0.00291
F3    4    0.102213    0.714054    0.397390    11.00000    0.02752    0.01966 =
         0.04799   -0.00881    0.02060   -0.00240
F4    4    0.539994    0.662917    0.566735    11.00000    0.05405    0.02460 =
         0.01453    0.00093   -0.00375   -0.01370
F5    4    0.651003    0.593151    0.307478    11.00000    0.02021    0.01562 =
         0.04708   -0.00205    0.01010    0.00381
N1    3    0.532670    0.765707    0.303545    11.00000    0.01859    0.01486 =
         0.01723    0.00107    0.00377    0.00078
N2    3    1.198565    0.932525    0.414091    11.00000    0.02048    0.01743 =
         0.02292   -0.00162    0.00471    0.00004
SB1   5    0.366759    0.647593    0.353616    11.00000    0.01866    0.01123 =
         0.01497   -0.00078    0.00319   -0.00226
HKLF 4

REM  final_a.res in P2(1)/n
REM R1 =  0.0402 for    1691 Fo > 4sig(Fo)  and  0.0573 for all    2112 data
REM    100 parameters refined using      0 restraints

END

WGHT      0.0474      3.0277

REM Highest difference peak  1.820,  deepest hole -1.064,  1-sigma level  0.241
Q1    1   0.5016  0.6457  0.3268  11.00000  0.05    1.82
Q2    1   0.2168  0.6495  0.3727  11.00000  0.05    1.68
Q3    1   0.3569  0.7230  0.3417  11.00000  0.05    1.33
Q4    1   0.3128  0.6449  0.2460  11.00000  0.05    1.11
Q5    1   0.3587  0.5689  0.3525  11.00000  0.05    0.92
;
_shelx_res_checksum              82909
####################################################################### 
# 
# 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_I_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1855722'
_audit_update_record             
;
2018-07-13 deposited with the CCDC.
2018-11-14 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C3 H2 As F5 N2'
_chemical_formula_iupac          ?
_chemical_formula_weight         235.99

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   5.3379(12)
_cell_length_b                   15.257(3)
_cell_length_c                   8.3529(18)
_cell_angle_alpha                90
_cell_angle_beta                 104.096(3)
_cell_angle_gamma                90
_cell_volume                     659.8(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9879
_cell_measurement_theta_min      2.6700
_cell_measurement_theta_max      30.5217
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear pale orange'
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.201
_exptl_crystal_size_min          0.168
_exptl_crystal_density_diffrn    2.376
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             448

_exptl_absorpt_coefficient_mu    5.185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5 (Bruker AXS, 2014)'
_exptl_absorpt_correction_T_min  0.31
_exptl_absorpt_correction_T_max  0.48

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'fine-focus tube'
_diffrn_source_type              ?

_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'

_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega- and phi-scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            15124
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_theta_min         2.67
_diffrn_reflns_theta_max         30.53
_diffrn_reflns_theta_full        30.53
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11

_refine_special_details          
;
;

_reflns_number_total             2017
_reflns_number_gt                1820
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0186
_refine_ls_wR_factor_gt          0.0411
_refine_ls_wR_factor_ref         0.0423
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_restrained_S_all      1.098
_refine_ls_number_reflns         2017
_refine_ls_number_parameters     100
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0185P)²+0.3482P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.435
_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'
N N 0.0061 0.0033 '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'

_computing_data_collection       
'Bruker Instrument Service v2012.12.0.3 (Bruker AXS, 2012)'
_computing_cell_refinement       'APEX2 v2014.11-0 (Bruker AXS, 2014)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS, 2013)'
_computing_structure_solution    'SHELXTL XT 2014/4 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXTL XL 2014/7 (Bruker AXS, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXTL XT 2014/4 (Bruker AXS, 2014)'

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
C C1 0.6134(3) 0.17312(10) 0.30272(17) 0.0132(3) Uani d . . . 1 . .
C C2 0.7097(3) 0.08390(9) 0.29131(18) 0.0138(2) Uani d . . . 1 . .
H H2A 0.6728 0.066 0.174 0.017 Uiso calc U . R 1 . .
H H2B 0.6184 0.0429 0.3495 0.017 Uiso calc U . R 1 . .
C C3 0.9894(3) 0.07839(9) 0.36433(17) 0.0136(3) Uani d . . . 1 . .
N N1 0.5352(2) 0.24145(8) 0.31238(14) 0.0145(2) Uani d . . . 1 . .
N N2 1.2053(2) 0.07138(8) 0.42217(16) 0.0183(2) Uani d . . . 1 . .
F F1 0.24070(19) 0.45079(6) 0.39682(12) 0.02214(19) Uani d . . . 1 . .
F F2 0.2295(2) 0.35720(6) 0.15175(12) 0.0263(2) Uani d . . . 1 . .
F F3 0.1338(2) 0.29324(7) 0.39457(16) 0.0341(3) Uani d . . . 1 . .
F F4 0.5449(2) 0.34172(7) 0.55678(12) 0.0345(3) Uani d . . . 1 . .
F F5 0.63934(18) 0.40563(6) 0.31565(14) 0.0277(2) Uani d . . . 1 . .
As As1 0.37744(3) 0.35517(2) 0.35626(2) 0.01272(5) Uani d . . . 1 . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
C1 0.0111(6) 0.0165(6) 0.0125(6) -0.0017(5) 0.0035(5) 0.0002(5)
C2 0.0130(6) 0.0119(6) 0.0174(6) 0.0006(5) 0.0056(5) -0.0006(5)
C3 0.0165(6) 0.0104(6) 0.0159(6) 0.0000(5) 0.0079(5) 0.0007(5)
N1 0.0138(5) 0.0147(6) 0.0148(5) 0.0002(4) 0.0034(4) 0.0000(4)
N2 0.0172(6) 0.0165(6) 0.0226(6) 0.0003(5) 0.0075(5) 0.0029(5)
F1 0.0285(5) 0.0150(4) 0.0238(5) 0.0088(4) 0.0081(4) -0.0004(3)
F2 0.0334(5) 0.0230(5) 0.0163(4) 0.0093(4) -0.0059(4) -0.0014(4)
F3 0.0282(5) 0.0196(5) 0.0637(8) 0.0033(4) 0.0294(5) 0.0078(5)
F4 0.0551(7) 0.0295(5) 0.0131(4) 0.0214(5) -0.0029(5) -0.0018(4)
F5 0.0204(5) 0.0155(4) 0.0494(6) -0.0018(4) 0.0129(4) 0.0002(4)
As1 0.01492(7) 0.01090(7) 0.01231(7) 0.00262(5) 0.00324(5) 0.00073(5)

_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
C1 N1 . 1.1333(19) ?
C1 C2 . 1.4664(19) ?
C2 C3 . 1.471(2) ?
C2 H2A . 0.99 ?
C2 H2B . 0.99 ?
C3 N2 . 1.1408(19) ?
N1 As1 . 2.0009(13) ?
F1 As1 . 1.7019(9) ?
F2 As1 . 1.6987(10) ?
F3 As1 . 1.6998(10) ?
F4 As1 . 1.7080(10) ?
F5 As1 . 1.7009(10) ?

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
N1 C1 C2 . . 178.76(15) ?
C1 C2 C3 . . 111.26(12) ?
C1 C2 H2A . . 109.4 ?
C3 C2 H2A . . 109.4 ?
C1 C2 H2B . . 109.4 ?
C3 C2 H2B . . 109.4 ?
H2A C2 H2B . . 108.0 ?
N2 C3 C2 . . 177.81(15) ?
C1 N1 As1 . . 171.70(12) ?
F2 As1 F3 . . 90.56(6) ?
F2 As1 F5 . . 89.69(6) ?
F3 As1 F5 . . 173.14(5) ?
F2 As1 F1 . . 93.88(5) ?
F3 As1 F1 . . 93.10(5) ?
F5 As1 F1 . . 93.72(5) ?
F2 As1 F4 . . 172.94(5) ?
F3 As1 F4 . . 89.44(6) ?
F5 As1 F4 . . 89.47(6) ?
F1 As1 F4 . . 93.17(5) ?
F2 As1 N1 . . 86.84(5) ?
F3 As1 N1 . . 85.86(5) ?
F5 As1 N1 . . 87.31(5) ?
F1 As1 N1 . . 178.75(5) ?
F4 As1 N1 . . 86.12(5) ?

_shelx_res_file                  
;
TITL first_a.res in P2(1)/n
CELL  0.71073   5.3379  15.2572   8.3529   90.000  104.096   90.000
ZERR    4.000   0.0012   0.0033   0.0018    0.000    0.003    0.000
LATT 1
SYMM 1/2-X, 1/2+Y, 1/2-Z
SFAC C  H  N  F  As
UNIT 12 8 8 20 4
LIST 4
L.S. 10
ACTA 58
CONF
BOND $H
FMAP 2
PLAN 5
SIZE 0.168 0.201 0.278
TEMP -173.140
WGHT    0.018500    0.348200
FVAR       0.54015
C1    1    0.613358    0.173115    0.302716    11.00000    0.01112    0.01648 =
         0.01249    0.00018    0.00354   -0.00170
C2    1    0.709699    0.083897    0.291309    11.00000    0.01304    0.01189 =
         0.01743   -0.00059    0.00557    0.00056
AFIX  23
H2A   2    0.672799    0.066015    0.173953    11.00000   -1.20000
H2B   2    0.618357    0.042925    0.349491    11.00000   -1.20000
AFIX   0
C3    1    0.989434    0.078387    0.364334    11.00000    0.01648    0.01042 =
         0.01587    0.00072    0.00787   -0.00001
N1    3    0.535162    0.241455    0.312377    11.00000    0.01380    0.01474 =
         0.01482    0.00004    0.00338    0.00020
N2    3    1.205303    0.071380    0.422168    11.00000    0.01721    0.01651 =
         0.02262    0.00290    0.00746    0.00027
F1    4    0.240699    0.450793    0.396820    11.00000    0.02848    0.01504 =
         0.02378   -0.00041    0.00807    0.00877
F2    4    0.229505    0.357200    0.151748    11.00000    0.03339    0.02305 =
         0.01633   -0.00139   -0.00590    0.00928
F3    4    0.133787    0.293245    0.394566    11.00000    0.02821    0.01965 =
         0.06374    0.00776    0.02938    0.00328
F4    4    0.544900    0.341717    0.556781    11.00000    0.05506    0.02954 =
         0.01305   -0.00184   -0.00285    0.02135
F5    4    0.639337    0.405631    0.315649    11.00000    0.02036    0.01553 =
         0.04944    0.00022    0.01290   -0.00184
AS1   5    0.377439    0.355172    0.356262    11.00000    0.01492    0.01090 =
         0.01231    0.00073    0.00324    0.00262
HKLF 4

REM  first_a.res in P2(1)/n
REM R1 =  0.0186 for    1820 Fo > 4sig(Fo)  and  0.0231 for all    2017 data
REM    100 parameters refined using      0 restraints

END

WGHT      0.0185      0.3482

REM Highest difference peak  0.286,  deepest hole -0.435,  1-sigma level  0.069
Q1    1   0.2977  0.3612  0.2406  11.00000  0.05    0.29
Q2    1   0.4746  0.2050  0.2752  11.00000  0.05    0.28
Q3    1   1.0927  0.0793  0.3393  11.00000  0.05    0.27
Q4    1   0.2450  0.4865  0.4071  11.00000  0.05    0.27
Q5    1   0.8351  0.0784  0.3175  11.00000  0.05    0.27
;
_shelx_res_checksum              1513
####################################################################### 
# 
# 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_TS383
_database_code_depnum_ccdc_archive 'CCDC 1855720'
_audit_update_record             
;
2018-07-13 deposited with the CCDC.
2018-11-14 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C8 H10 As2 F10 N2'
_chemical_formula_sum            'C8 H10 As2 F10 N2'
_chemical_formula_iupac          ?
_chemical_formula_weight         474.02

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/m 1'
_space_group_name_Hall           '-P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   5.227(5)
_cell_length_b                   8.481(7)
_cell_length_c                   8.215(7)
_cell_angle_alpha                90
_cell_angle_beta                 100.370(12)
_cell_angle_gamma                90
_cell_volume                     358.2(5)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    139
_cell_measurement_theta_min      2.5497
_cell_measurement_theta_max      26.2330
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_size_max          0.402
_exptl_crystal_size_mid          0.328
_exptl_crystal_size_min          0.225
_exptl_crystal_density_diffrn    2.197
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             228

_exptl_absorpt_coefficient_mu    4.772
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   'SADABS 2014/5 (Bruker AXS, 2014)'
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4392

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'fine-focus tube'
_diffrn_source_type              ?

_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'

_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega- and phi-scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            8928
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_theta_min         2.52
_diffrn_reflns_theta_max         30.65
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11

_refine_special_details          
;
;

_reflns_number_total             1148
_reflns_number_gt                1025
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0249
_refine_ls_wR_factor_gt          0.0478
_refine_ls_wR_factor_ref         0.0490
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_restrained_S_all      1.096
_refine_ls_number_reflns         1148
_refine_ls_number_parameters     58
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0136P)²+0.1813P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.753
_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'
As As 0.0499 2.0058 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       
'Bruker Instrument Service v2012.12.0.3 (Bruker AXS, 2012)'
_computing_cell_refinement       'APEX2 v2014.11-0 (Bruker AXS, 2014)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS, 2013)'
_computing_structure_solution    'SHELXTL XT 2014/4 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXTL XL 2014/7 (Bruker AXS, 2014)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 807)'
_computing_publication_material  'SHELXTL XT 2014/4 (Bruker AXS, 2014)'

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
C C1 0.3754(4) 0.75 0.6427(3) 0.0183(5) Uani d T P S 1 . .
C C2 0.3094(5) 0.75 0.8032(3) 0.0202(5) Uani d T P S 1 . .
H H2 0.4586 0.75 0.8984 0.024 Uiso calc U P R 1 . .
C C3 0.0663(4) 0.6629(2) 0.8303(3) 0.0236(4) Uani d . . . 1 . .
H H3A -0.0383 0.6086 0.7341 0.028 Uiso calc U . R 1 . .
H H3B 0.0719 0.6086 0.9376 0.028 Uiso calc U . R 1 . .
As As1 0.60080(5) 0.75 0.31950(3) 0.01407(8) Uani d T P S 1 . .
F F1 0.7483(3) 0.75 0.1509(2) 0.0274(4) Uani d T P S 1 . .
F F2 0.3852(2) 0.60751(15) 0.23790(16) 0.0352(3) Uani d . . . 1 . .
F F3 0.8041(2) 0.89142(13) 0.41862(15) 0.0290(3) Uani d . . . 1 . .
N N1 0.4368(4) 0.75 0.5164(3) 0.0188(4) Uani d T P S 1 . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
C1 0.0158(11) 0.0164(11) 0.0213(14) 0 0.0000(10) 0
C2 0.0191(11) 0.0250(13) 0.0161(13) 0 0.0018(9) 0
C3 0.0288(10) 0.0215(9) 0.0227(10) -0.0041(7) 0.0108(8) 0.0013(7)
As1 0.01376(11) 0.01459(12) 0.01349(13) 0 0.00143(8) 0
F1 0.0244(8) 0.0428(10) 0.0165(8) 0 0.0077(6) 0
F2 0.0342(6) 0.0425(7) 0.0288(7) -0.0195(6) 0.0056(5) -0.0158(6)
F3 0.0327(6) 0.0292(6) 0.0258(7) -0.0155(5) 0.0069(5) -0.0058(5)
N1 0.0167(9) 0.0220(11) 0.0185(12) 0 0.0054(8) 0

_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
C1 N1 . 1.140(4) ?
C1 C2 . 1.422(4) ?
C2 C3 4_575 1.521(3) ?
C2 C3 . 1.521(3) ?
C2 H2 . 1.0 ?
C3 C3 4_575 1.478(4) ?
C3 H3A . 0.99 ?
C3 H3B . 0.99 ?
As1 F1 . 1.702(2) ?
As1 F2 . 1.7051(15) ?
As1 F2 4_575 1.7051(15) ?
As1 F3 . 1.7085(14) ?
As1 F3 4_575 1.7085(14) ?
As1 N1 . 1.962(3) ?

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
N1 C1 C2 . . 177.7(3) ?
C1 C2 C3 . 4_575 118.97(19) ?
C1 C2 C3 . . 118.98(19) ?
C3 C2 C3 4_575 . 58.15(18) ?
C1 C2 H2 . . 116.1 ?
C3 C2 H2 4_575 . 116.1 ?
C3 C2 H2 . . 116.1 ?
C3 C3 C2 4_575 . 60.93(9) ?
C3 C3 H3A 4_575 . 117.7 ?
C2 C3 H3A . . 117.7 ?
C3 C3 H3B 4_575 . 117.7 ?
C2 C3 H3B . . 117.7 ?
H3A C3 H3B . . 114.8 ?
F1 As1 F2 . . 92.53(7) ?
F1 As1 F2 . 4_575 92.53(7) ?
F2 As1 F2 . 4_575 90.26(12) ?
F1 As1 F3 . . 93.09(7) ?
F2 As1 F3 . . 174.36(6) ?
F2 As1 F3 4_575 . 90.01(9) ?
F1 As1 F3 . 4_575 93.09(7) ?
F2 As1 F3 . 4_575 90.01(9) ?
F2 As1 F3 4_575 4_575 174.36(6) ?
F3 As1 F3 . 4_575 89.17(10) ?
F1 As1 N1 . . 179.00(8) ?
F2 As1 N1 . . 88.18(8) ?
F2 As1 N1 4_575 . 88.18(8) ?
F3 As1 N1 . . 86.19(8) ?
F3 As1 N1 4_575 . 86.19(8) ?
C1 N1 As1 . . 170.6(2) ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C1 C2 C3 C3 . . . 4_575 -107.93(16) ?

_shelx_res_file                  
;


    final_a.res created by SHELXL-2014/7


TITL final_a.res in P2(1)/m
REM Old TITL final in P2(1)/m
REM SHELXT solution in P2(1)/m
REM R1 0.107,  Rweak 0.010,  Alpha 0.046,  Orientation as input
REM Formula found by SHELXT:  C9 As N
CELL  0.71073   5.2268   8.4809   8.2150   90.000  100.370   90.000
ZERR    1.000   0.0045   0.0072   0.0070    0.000    0.012    0.000
LATT  1
SYMM -X, 1/2+Y, -Z
SFAC C H AS F N
UNIT 8 10 2 10 2
TEMP -173.140
L.S. 10
BOND $H
LIST 4
ACTA 55
CONF
FMAP 2
PLAN 20
WGHT    0.013600    0.181300
FVAR       0.97572
C1    1    0.375425    0.750000    0.642700    10.50000    0.01583    0.01643 =
         0.02126    0.00000    0.00003    0.00000
C2    1    0.309427    0.750000    0.803234    10.50000    0.01913    0.02497 =
         0.01610    0.00000    0.00180    0.00000
AFIX  13
H2    2    0.458611    0.750000    0.898424    10.50000   -1.20000
AFIX   0
C3    1    0.066290    0.662866    0.830338    11.00000    0.02880    0.02149 =
         0.02272    0.00127    0.01081   -0.00413
AFIX  23
H3A   2   -0.038279    0.608646    0.734060    11.00000   -1.20000
H3B   2    0.071906    0.608647    0.937647    11.00000   -1.20000
AFIX   0
AS1   3    0.600795    0.750000    0.319498    10.50000    0.01376    0.01459 =
         0.01349    0.00000    0.00143    0.00000
F1    4    0.748253    0.750000    0.150898    10.50000    0.02436    0.04285 =
         0.01653    0.00000    0.00769    0.00000
F2    4    0.385225    0.607509    0.237900    11.00000    0.03424    0.04251 =
         0.02882   -0.01579    0.00561   -0.01947
F3    4    0.804079    0.891415    0.418616    11.00000    0.03271    0.02923 =
         0.02582   -0.00577    0.00691   -0.01554
N1    5    0.436811    0.750000    0.516373    10.50000    0.01666    0.02204 =
         0.01853    0.00000    0.00537    0.00000
HKLF 4

REM  final_a.res in P2(1)/m
REM R1 =  0.0249 for    1025 Fo > 4sig(Fo)  and  0.0315 for all    1148 data
REM     58 parameters refined using      0 restraints

END

WGHT      0.0136      0.1813

REM Highest difference peak  0.456,  deepest hole -0.753,  1-sigma level  0.103
Q1    1  -0.0655  0.7500  0.6283  10.50000  0.05    0.46
Q2    1  -0.0021  0.7500  0.8725  10.50000  0.05    0.45
Q3    1   0.5437  0.7500  0.4546  10.50000  0.05    0.45
Q4    1   0.6365  0.7500  0.1850  10.50000  0.05    0.44
Q5    1   0.6378  0.7500  0.6374  10.50000  0.05    0.38
Q6    1   0.8894  0.7500  0.0629  10.50000  0.05    0.36
Q7    1   0.2100  0.7500  0.1618  10.50000  0.05    0.33
Q8    1   0.1965  0.6989  0.8219  11.00000  0.05    0.33
Q9    1   0.5147  0.7500  0.5572  10.50000  0.05    0.32
Q10   1   0.3162  0.7500  1.0054  10.50000  0.05    0.31
Q11   1   0.3554  0.5900  0.3487  11.00000  0.05    0.31
Q12   1   0.8215  0.8120  0.3906  11.00000  0.05    0.30
Q13   1   0.6742  0.9287  0.4804  11.00000  0.05    0.30
Q14   1   0.6353  0.8439  0.9282  11.00000  0.05    0.30
Q15   1   0.2371  0.4343  0.9951  11.00000  0.05    0.29
Q16   1   0.5333  0.5811  0.1450  11.00000  0.05    0.29
Q17   1   0.9584  0.8329  0.3366  11.00000  0.05    0.28
Q18   1   0.2571  0.5571  1.0472  11.00000  0.05    0.28
Q19   1   0.4177  0.7500  0.8460  10.50000  0.05    0.28
Q20   1   0.8642  0.7706  0.5252  11.00000  0.05    0.28
;
_shelx_res_checksum              61284
