# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_2ayt83
_database_code_depnum_ccdc_archive 'CCDC 2086686'
loop_
_audit_author_name
_audit_author_address
'Alexander Virovets'
;University of Regensburg
Germany
;
_audit_update_record             
;
2021-05-29 deposited with the CCDC.	2021-08-17 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT094_2ayt83              
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       2.89 Report
RESPONSE: The structure shows very peculiar disorder: the whole molecule 
is shifted by (0, 0, 1/2) vector with relative weight of two positions of 
~99%/1%. Our attempt to refine this disorder failed because of its very low
contribution to the diffraction.
;
_vrf_PLAT971_2ayt83              
;
PROBLEM: Check Calcd Resid. Dens.  1.68A   From F3              2.01 eA-3  
RESPONSE: This peak corresponds to the very minor (~1%) second position of 
central Sb atom corresponding to the whole molecule shifted by (0, 0, 1/2) 
vector. 
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C5 H5 F5 N Sb'
_chemical_formula_weight         295.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.0562 5.8946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+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                   7.3140(7)
_cell_length_b                   15.8817(12)
_cell_length_c                   7.2618(9)
_cell_angle_alpha                90
_cell_angle_beta                 104.291(11)
_cell_angle_gamma                90
_cell_volume                     817.42(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    976
_cell_measurement_theta_min      5.5530
_cell_measurement_theta_max      72.6720
_cell_measurement_temperature    123(2)

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 6 0 0.0441
-4 -5 0 0.0052
0 10 -1 0.0311
0 -10 1 0.0311
1 -10 -1 0.0330
-1 10 1 0.0330
2 2 -5 0.0618
-2 6 4 0.0418
2 -6 -4 0.0418
-1 2 -4 0.0476
1 -2 4 0.0476

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_absorpt_correction_T_min  0.159
_exptl_absorpt_correction_T_max  0.410
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_density_diffrn    2.404
_exptl_crystal_F_000             552
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.103
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.052
_exptl_absorpt_coefficient_mu    27.215
_shelx_estimated_absorpt_T_min   0.166
_shelx_estimated_absorpt_T_max   0.332

_diffrn_ambient_temperature      123(2)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
_diffrn_detector_area_resol_mean 5.2548
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            1335
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_av_R_equivalents  0.0161
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         5.571
_diffrn_reflns_theta_max         73.352
_diffrn_reflns_theta_full        67.500
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             796
_reflns_number_gt                753
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    SHELXT
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0669P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         796
_refine_ls_number_parameters     57
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0329
_refine_ls_wR_factor_ref         0.0821
_refine_ls_wR_factor_gt          0.0816
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb 0.500000 0.16143(2) 0.250000 0.0240(2) Uani 1 2 d S T P . .
F1 F 0.7644(5) 0.16258(17) 0.3389(5) 0.0350(7) Uani 1 1 d . . . . .
F2 F 0.500000 0.0438(3) 0.250000 0.0422(11) Uani 1 2 d S T P . .
F3 F 0.4761(5) 0.16433(17) 0.5012(5) 0.0303(6) Uani 1 1 d . . . . .
N1 N 0.500000 0.2933(3) 0.250000 0.0233(11) Uani 1 2 d S T P . .
C1 C 0.6402(8) 0.3356(3) 0.1979(8) 0.0312(11) Uani 1 1 d . . . . .
H1A H 0.737990 0.305055 0.162622 0.037 Uiso 1 1 calc R U . . .
C2 C 0.6425(8) 0.4222(4) 0.1954(8) 0.0385(12) Uani 1 1 d . . . . .
H2A H 0.739742 0.451777 0.157023 0.046 Uiso 1 1 calc R U . . .
C3 C 0.500000 0.4654(5) 0.250000 0.0403(18) Uani 1 2 d S T P . .
H3A H 0.499999 0.525187 0.249999 0.048 Uiso 1 2 calc R U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sb1 0.0189(3) 0.0227(3) 0.0309(3) 0.000 0.00680(17) 0.000
F1 0.0237(15) 0.0345(17) 0.0463(19) 0.0013(11) 0.0076(14) 0.0030(10)
F2 0.036(2) 0.0211(18) 0.069(3) 0.000 0.011(2) 0.000
F3 0.0288(16) 0.0321(16) 0.0313(15) 0.0072(9) 0.0097(13) -0.0003(9)
N1 0.019(2) 0.025(3) 0.024(3) 0.000 0.003(2) 0.000
C1 0.029(3) 0.030(3) 0.036(3) -0.0002(17) 0.009(2) -0.0062(16)
C2 0.038(3) 0.033(3) 0.041(3) 0.006(2) 0.004(2) -0.011(2)
C3 0.053(5) 0.024(4) 0.035(4) 0.000 -0.005(4) 0.000

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sb1 F2 1.868(4) . ?
Sb1 F3 1.876(3) 2_655 ?
Sb1 F3 1.876(3) . ?
Sb1 F1 1.882(3) 2_655 ?
Sb1 F1 1.882(3) . ?
Sb1 N1 2.095(5) . ?
N1 C1 1.355(6) 2_655 ?
N1 C1 1.355(6) . ?
C1 C2 1.376(7) . ?
C1 H1A 0.9500 . ?
C2 C3 1.384(7) . ?
C2 H2A 0.9500 . ?
C3 H3A 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F2 Sb1 F3 91.41(8) . 2_655 ?
F2 Sb1 F3 91.41(8) . . ?
F3 Sb1 F3 177.19(17) 2_655 . ?
F2 Sb1 F1 90.56(8) . 2_655 ?
F3 Sb1 F1 90.03(15) 2_655 2_655 ?
F3 Sb1 F1 89.94(15) . 2_655 ?
F2 Sb1 F1 90.56(8) . . ?
F3 Sb1 F1 89.94(15) 2_655 . ?
F3 Sb1 F1 90.03(15) . . ?
F1 Sb1 F1 178.89(16) 2_655 . ?
F2 Sb1 N1 180.0 . . ?
F3 Sb1 N1 88.59(8) 2_655 . ?
F3 Sb1 N1 88.59(8) . . ?
F1 Sb1 N1 89.44(8) 2_655 . ?
F1 Sb1 N1 89.44(8) . . ?
C1 N1 C1 120.7(6) 2_655 . ?
C1 N1 Sb1 119.7(3) 2_655 . ?
C1 N1 Sb1 119.7(3) . . ?
N1 C1 C2 120.7(5) . . ?
N1 C1 H1A 119.6 . . ?
C2 C1 H1A 119.6 . . ?
C1 C2 C3 118.6(5) . . ?
C1 C2 H2A 120.7 . . ?
C3 C2 H2A 120.7 . . ?
C2 C3 C2 120.6(7) 2_655 . ?
C2 C3 H3A 119.7 2_655 . ?
C2 C3 H3A 119.7 . . ?

_refine_diff_density_max         2.101
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.178

_shelx_res_file                  
;

TITL ayt83 in C2/c at 123K Gemini XT-solved
    83.res
    created by SHELXL-2018/3 at 15:51:21 on 23-Jul-2019
CELL 1.54178   7.3140  15.8817   7.2618  90.000 104.291  90.000
ZERR    4.00   0.0007   0.0012   0.0009   0.000   0.011   0.000
LATT  7
SYMM -X, Y, 0.5-Z
SFAC C H N F SB
UNIT 20 20 4 20 4
TEMP -150

L.S. 10
PLAN  20
BOND $H
fmap 2
ACTA 135
SIZE 0.103 0.091 0.052

WGHT    0.066900
FVAR       0.11319
SB1   5    0.500000    0.161433    0.250000    10.50000    0.01891    0.02269 =
         0.03086    0.00000    0.00680    0.00000
F1    4    0.764400    0.162581    0.338907    11.00000    0.02368    0.03448 =
         0.04634    0.00129    0.00761    0.00298
F2    4    0.500000    0.043844    0.250000    10.50000    0.03600    0.02110 =
         0.06875    0.00000    0.01128    0.00000
F3    4    0.476140    0.164333    0.501215    11.00000    0.02885    0.03214 =
         0.03126    0.00724    0.00973   -0.00029
N1    3    0.500000    0.293338    0.250000    10.50000    0.01943    0.02523 =
         0.02410    0.00000    0.00314    0.00000
C1    1    0.640196    0.335582    0.197859    11.00000    0.02864    0.02994 =
         0.03560   -0.00020    0.00930   -0.00620
AFIX  43
H1A   2    0.737990    0.305055    0.162622    11.00000   -1.20000
AFIX   0
C2    1    0.642451    0.422204    0.195397    11.00000    0.03832    0.03343 =
         0.04101    0.00605    0.00433   -0.01095
AFIX  43
H2A   2    0.739742    0.451777    0.157023    11.00000   -1.20000
AFIX   0
C3    1    0.500000    0.465370    0.250000    10.50000    0.05331    0.02386 =
         0.03541    0.00000   -0.00483    0.00000
AFIX  43
H3A   2    0.499999    0.525187    0.249999    10.50000   -1.20000

AFIX   0
HKLF 4




REM  ayt83 in C2/c at 123K Gemini XT-solved
REM wR2 = 0.0821, GooF = S = 1.037, Restrained GooF = 1.037 for all data
REM R1 = 0.0329 for 753 Fo > 4sig(Fo) and 0.0343 for all 796 data
REM 57 parameters refined using 0 restraints

END

WGHT      0.0669      0.0000

REM Highest difference peak  2.101,  deepest hole -0.728,  1-sigma level  0.178
Q1    1   0.5000  0.1607  0.7500  10.50000  0.05    2.10
Q2    1   0.4209  0.1671  0.1402  11.00000  0.05    0.88
Q3    1   0.4408  0.1223  0.1918  11.00000  0.05    0.84
Q4    1   0.6840  0.1614  0.5061  11.00000  0.05    0.53
Q5    1   0.7361  0.3304 -0.0211  11.00000  0.05    0.52
Q6    1   0.7057  0.1616  0.2974  11.00000  0.05    0.50
Q7    1   0.7131  0.1575  0.1707  11.00000  0.05    0.49
Q8    1   0.8034  0.1881  0.2920  11.00000  0.05    0.42
Q9    1   0.7923  0.1550  0.5579  11.00000  0.05    0.40
Q10   1   0.5063  0.3223  0.0469  11.00000  0.05    0.36
Q11   1   0.4818  0.2308  0.5073  11.00000  0.05    0.35
Q12   1   0.4641  0.0854  0.5039  11.00000  0.05    0.35
Q13   1   0.8531  0.1735  0.1400  11.00000  0.05    0.34
Q14   1   0.7619  0.3225  0.2538  11.00000  0.05    0.32
Q15   1   0.3774  0.2830  0.1932  11.00000  0.05    0.29
Q16   1   0.4951  0.0286  0.0468  11.00000  0.05    0.29
Q17   1   0.9622  0.1659  0.2980  11.00000  0.05    0.29
Q18   1   0.5426  0.3110  0.2211  11.00000  0.05    0.28
Q19   1   0.8126  0.1019  0.3980  11.00000  0.05    0.28
Q20   1   0.6604  0.3823  0.2208  11.00000  0.05    0.27
;
_shelx_res_checksum              66276

_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_4ayt85
_database_code_depnum_ccdc_archive 'CCDC 2086689'
loop_
_audit_author_name
_audit_author_address
'Alexander Virovets'
;University of Regensburg
Germany
;
_audit_update_record             
;
2021-05-29 deposited with the CCDC.	2021-08-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ' C5 H6 N, F4 Sb, F3 Sb'
_chemical_formula_sum            'C5 H6 F7 N Sb2'
_chemical_formula_weight         456.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.0562 5.8946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-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                   9.87611(18)
_cell_length_b                   8.40553(15)
_cell_length_c                   24.6121(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2043.15(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3333
_cell_measurement_theta_min      3.5570
_cell_measurement_theta_max      73.7620

_exptl_crystal_description       'elongated prism'
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.969
_exptl_crystal_F_000             1664
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.102
_exptl_crystal_size_mid          0.042
_exptl_crystal_size_min          0.017

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 0 0.0291
0 0 1 0.0085
0 0 -1 0.0090
0 -1 1 0.0502
1 0 0 0.0127
0 1 -1 0.0410

_exptl_absorpt_coefficient_mu    42.723
_shelx_estimated_absorpt_T_min   0.097
_shelx_estimated_absorpt_T_max   0.530
_exptl_absorpt_correction_T_min  0.137
_exptl_absorpt_correction_T_max  0.541
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.21a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_ambient_environment      N~2~
_diffrn_source_type              'microfocus SuperNova source'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            TitanS2
_diffrn_detector_area_resol_mean 4.2047
_diffrn_reflns_number            6189
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         3.592
_diffrn_reflns_theta_max         73.938
_diffrn_reflns_theta_full        67.500
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2065
_reflns_number_gt                1703
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0342P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2065
_refine_ls_number_parameters     136
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0246
_refine_ls_wR_factor_ref         0.0557
_refine_ls_wR_factor_gt          0.0542
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_restrained_S_all      0.927
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb 0.55194(3) 0.41958(3) 0.75214(2) 0.01419(9) Uani 1 1 d . . . . .
F1 F 0.3699(3) 0.3781(4) 0.72814(12) 0.0228(6) Uani 1 1 d . . . . .
F2 F 0.5851(3) 0.4512(4) 0.66806(10) 0.0202(6) Uani 1 1 d . . . . .
F3 F 0.6037(3) 0.2042(3) 0.73371(12) 0.0219(6) Uani 1 1 d . . . . .
F4 F 0.4908(3) 0.3114(4) 0.82198(13) 0.0280(7) Uani 1 1 d . . . . .
Sb2 Sb 0.27077(3) 0.27528(3) 0.87862(2) 0.01348(9) Uani 1 1 d . . . . .
F5 F 0.3264(3) 0.4934(3) 0.89565(12) 0.0198(6) Uani 1 1 d . . . . .
F6 F 0.3947(3) 0.2069(4) 0.93432(11) 0.0200(5) Uani 1 1 d . . . . .
F7 F 0.1332(3) 0.3012(4) 0.93422(11) 0.0195(5) Uani 1 1 d . . . . .
N1 N 0.3679(4) 0.5312(6) 0.60513(19) 0.0268(10) Uani 1 1 d . . . . .
H1 H 0.448507 0.521642 0.620048 0.032 Uiso 1 1 calc R U . . .
C1 C 0.3508(5) 0.4772(7) 0.5543(2) 0.0270(11) Uani 1 1 d . . . . .
H1A H 0.424325 0.431056 0.535043 0.032 Uiso 1 1 calc R U . . .
C2 C 0.2249(5) 0.4896(7) 0.5305(2) 0.0269(11) Uani 1 1 d . . . . .
H2 H 0.210326 0.451697 0.494622 0.032 Uiso 1 1 calc R U . . .
C3 C 0.1201(5) 0.5580(8) 0.5596(2) 0.0276(12) Uani 1 1 d . . . . .
H3 H 0.032696 0.566789 0.543819 0.033 Uiso 1 1 calc R U . . .
C4 C 0.1428(6) 0.6134(7) 0.6117(2) 0.0252(11) Uani 1 1 d . . . . .
H4 H 0.071384 0.661312 0.631770 0.030 Uiso 1 1 calc R U . . .
C5 C 0.2695(6) 0.5988(7) 0.6343(2) 0.0265(11) Uani 1 1 d . . . . .
H5 H 0.286798 0.636011 0.670122 0.032 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sb1 0.01201(13) 0.01372(15) 0.01684(14) -0.00077(11) 0.00013(10) -0.00026(10)
F1 0.0116(12) 0.0229(16) 0.0339(14) -0.0019(12) -0.0022(11) -0.0021(11)
F2 0.0184(13) 0.0232(15) 0.0190(11) 0.0017(11) -0.0010(10) 0.0029(11)
F3 0.0221(14) 0.0108(13) 0.0330(14) -0.0017(11) 0.0029(11) 0.0008(11)
F4 0.0199(14) 0.037(2) 0.0269(14) 0.0055(13) 0.0032(12) 0.0015(13)
Sb2 0.01132(14) 0.01300(15) 0.01612(13) 0.00004(10) 0.00059(9) 0.00082(10)
F5 0.0160(13) 0.0146(14) 0.0289(13) 0.0010(11) -0.0004(10) -0.0011(11)
F6 0.0166(13) 0.0231(15) 0.0204(12) 0.0010(11) -0.0004(10) 0.0020(11)
F7 0.0156(12) 0.0197(15) 0.0232(12) -0.0004(11) 0.0053(10) 0.0011(11)
N1 0.0124(19) 0.034(3) 0.034(2) 0.0116(19) -0.0075(16) -0.0079(18)
C1 0.017(2) 0.029(3) 0.035(3) 0.011(2) 0.007(2) 0.006(2)
C2 0.021(3) 0.039(3) 0.020(2) -0.002(2) -0.0005(18) 0.006(2)
C3 0.016(2) 0.043(4) 0.025(2) -0.007(2) -0.0023(19) 0.003(2)
C4 0.024(3) 0.031(3) 0.020(2) 0.002(2) 0.0002(19) 0.001(2)
C5 0.030(3) 0.025(3) 0.025(2) 0.003(2) -0.007(2) -0.011(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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sb1 F1 1.924(3) . ?
Sb1 F3 1.935(3) . ?
Sb1 F4 2.036(3) . ?
Sb1 F2 2.112(3) . ?
F2 Sb2 2.621(3) 6_657 ?
F4 Sb2 2.600(3) . ?
Sb2 F6 1.926(3) . ?
Sb2 F7 1.940(3) . ?
Sb2 F5 1.960(3) . ?
Sb2 F5 2.590(3) 8_655 ?
N1 C5 1.336(8) . ?
N1 C1 1.341(8) . ?
N1 H1 0.8800 . ?
C1 C2 1.378(8) . ?
C1 H1A 0.9500 . ?
C2 C3 1.384(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.383(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.375(8) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F1 Sb1 F3 90.32(13) . . ?
F1 Sb1 F4 84.34(13) . . ?
F3 Sb1 F4 81.87(14) . . ?
F1 Sb1 F2 82.35(12) . . ?
F3 Sb1 F2 81.19(12) . . ?
F4 Sb1 F2 158.34(13) . . ?
Sb1 F2 Sb2 117.85(12) . 6_657 ?
Sb1 F4 Sb2 138.82(15) . . ?
F6 Sb2 F7 88.66(11) . . ?
F6 Sb2 F5 87.07(13) . . ?
F7 Sb2 F5 86.58(12) . . ?
F6 Sb2 F5 81.22(11) . 8_655 ?
F7 Sb2 F5 74.30(11) . 8_655 ?
F5 Sb2 F5 157.70(14) . 8_655 ?
F6 Sb2 F4 83.40(10) . . ?
F7 Sb2 F4 161.84(12) . . ?
F5 Sb2 F4 76.75(12) . . ?
F5 Sb2 F4 120.23(10) 8_655 . ?
F6 Sb2 F2 157.71(11) . 6_557 ?
F7 Sb2 F2 75.87(10) . 6_557 ?
F5 Sb2 F2 76.24(10) . 6_557 ?
F5 Sb2 F2 109.12(9) 8_655 6_557 ?
F4 Sb2 F2 106.49(10) . 6_557 ?
Sb2 F5 Sb2 135.84(13) . 8_665 ?
C5 N1 C1 123.7(4) . . ?
C5 N1 H1 118.2 . . ?
C1 N1 H1 118.2 . . ?
N1 C1 C2 119.0(5) . . ?
N1 C1 H1A 120.5 . . ?
C2 C1 H1A 120.5 . . ?
C1 C2 C3 119.1(5) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 H2 120.5 . . ?
C4 C3 C2 119.9(5) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C5 C4 C3 119.5(5) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
N1 C5 C4 118.9(5) . . ?
N1 C5 H5 120.6 . . ?
C4 C5 H5 120.6 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1 F2 0.88 1.89 2.730(5) 159.3 . yes
C1 H1A F7 0.95 2.45 3.169(6) 132.1 6_657 yes
C2 H2 F5 0.95 2.51 3.361(6) 149.8 2_564 yes

_refine_diff_density_max         0.639
_refine_diff_density_min         -1.565
_refine_diff_density_rms         0.175

_shelx_res_file                  
;
TITL ayt85 in Pbca at 100K newGV
    85.res
    created by SHELXL-2018/3 at 16:48:36 on 06-Sep-2019
CELL 1.54178   9.87611   8.40553  24.61212  90.0000  90.0000  90.0000
ZERR    8.00   0.00018   0.00015   0.00041   0.0000   0.0000   0.0000
LATT  1
SYMM 0.5-X, -Y, 0.5+Z
SYMM -X, 0.5+Y, 0.5-Z
SYMM 0.5+X, 0.5-Y, -Z
SFAC C H N F SB
UNIT 40 48 8 56 16

L.S. 10
PLAN  20
SIZE 0.102 0.042 0.017
TEMP -173
CONN 12 1.6 $Sb
OMIT 6 9 0
HTAB N1 F2
EQIV $2 x+1/2, y, -z+3/2
HTAB C1 F7_$2
EQIV $5 -x+1/2, -y+1, z-1/2
HTAB C2 F5_$5

BOND $H
fmap 2
acta 135

WGHT    0.034200
FVAR       0.04822
SB1   5    0.551943    0.419577    0.752143    11.00000    0.01201    0.01372 =
         0.01684   -0.00077    0.00013   -0.00026
F1    4    0.369877    0.378138    0.728140    11.00000    0.01158    0.02292 =
         0.03391   -0.00187   -0.00219   -0.00214
F2    4    0.585111    0.451175    0.668061    11.00000    0.01840    0.02324 =
         0.01901    0.00174   -0.00103    0.00293
F3    4    0.603712    0.204180    0.733705    11.00000    0.02209    0.01077 =
         0.03297   -0.00173    0.00287    0.00082
F4    4    0.490847    0.311443    0.821981    11.00000    0.01986    0.03720 =
         0.02695    0.00549    0.00317    0.00153
SB2   5    0.270774    0.275281    0.878623    11.00000    0.01132    0.01300 =
         0.01612    0.00004    0.00059    0.00082
F5    4    0.326418    0.493427    0.895647    11.00000    0.01602    0.01460 =
         0.02889    0.00104   -0.00044   -0.00108
F6    4    0.394742    0.206889    0.934323    11.00000    0.01656    0.02310 =
         0.02042    0.00103   -0.00042    0.00200
F7    4    0.133222    0.301230    0.934215    11.00000    0.01562    0.01970 =
         0.02323   -0.00039    0.00535    0.00113
N1    3    0.367942    0.531215    0.605128    11.00000    0.01242    0.03364 =
         0.03423    0.01157   -0.00751   -0.00786
AFIX  43
H1    2    0.448507    0.521642    0.620048    11.00000   -1.20000
AFIX   0
C1    1    0.350820    0.477176    0.554326    11.00000    0.01653    0.02948 =
         0.03488    0.01125    0.00726    0.00608
AFIX  43
H1A   2    0.424325    0.431056    0.535043    11.00000   -1.20000
AFIX   0
C2    1    0.224934    0.489571    0.530513    11.00000    0.02113    0.03925 =
         0.02017   -0.00198   -0.00051    0.00576
AFIX  43
H2    2    0.210326    0.451697    0.494622    11.00000   -1.20000
AFIX   0
C3    1    0.120136    0.557955    0.559620    11.00000    0.01560    0.04261 =
         0.02457   -0.00700   -0.00233    0.00302
AFIX  43
H3    2    0.032696    0.566789    0.543819    11.00000   -1.20000
AFIX   0
C4    1    0.142806    0.613436    0.611742    11.00000    0.02414    0.03140 =
         0.02000    0.00183    0.00023    0.00145
AFIX  43
H4    2    0.071384    0.661312    0.631770    11.00000   -1.20000
AFIX   0
C5    1    0.269542    0.598755    0.634344    11.00000    0.02954    0.02472 =
         0.02528    0.00337   -0.00723   -0.01136
AFIX  43
H5    2    0.286798    0.636011    0.670122    11.00000   -1.20000

AFIX   0
HKLF 4




REM  ayt85 in Pbca at 100K newGV
REM wR2 = 0.0557, GooF = S = 0.927, Restrained GooF = 0.927 for all data
REM R1 = 0.0246 for 1703 Fo > 4sig(Fo) and 0.0323 for all 2065 data
REM 136 parameters refined using 0 restraints

END

WGHT      0.0342      0.0000

REM Highest difference peak  0.639,  deepest hole -1.565,  1-sigma level  0.175
Q1    1   0.6159  0.3063  0.7554  11.00000  0.05    0.64
Q2    1   0.6592  0.5547  0.6917  11.00000  0.05    0.61
Q3    1   0.4807  0.3162  0.7579  11.00000  0.05    0.57
Q4    1   0.4360  0.3929  0.7093  11.00000  0.05    0.51
Q5    1   0.3343  0.4772  0.9409  11.00000  0.05    0.50
Q6    1   0.4561  0.4331  0.6309  11.00000  0.05    0.50
Q7    1   0.6366  0.2436  0.6770  11.00000  0.05    0.49
Q8    1   0.6006  0.6173  0.6805  11.00000  0.05    0.49
Q9    1   0.6921  0.4746  0.6735  11.00000  0.05    0.48
Q10   1   0.3393  0.1705  0.8643  11.00000  0.05    0.47
Q11   1   0.2577  0.5544  0.8312  11.00000  0.05    0.47
Q12   1   0.6166  0.5272  0.7821  11.00000  0.05    0.47
Q13   1   0.5802  0.0710  0.7006  11.00000  0.05    0.46
Q14   1   0.5807  0.2022  0.8193  11.00000  0.05    0.46
Q15   1   0.3384  0.3867  0.8023  11.00000  0.05    0.46
Q16   1   0.4410  0.3013  0.9318  11.00000  0.05    0.46
Q17   1   0.6759  0.4442  0.8019  11.00000  0.05    0.45
Q18   1   0.4217  0.5721  0.7013  11.00000  0.05    0.45
Q19   1   0.3393  0.1883  0.9014  11.00000  0.05    0.45
Q20   1   0.4530  0.5190  0.7089  11.00000  0.05    0.45
;
_shelx_res_checksum              22101

_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_1ayt88
_database_code_depnum_ccdc_archive 'CCDC 2086688'
loop_
_audit_author_name
_audit_author_address
'Alexander Virovets'
;University of Regensburg
Germany
;
_audit_update_record             
;
2021-05-29 deposited with the CCDC.	2021-08-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H3 F10 N Sb2'
_chemical_formula_sum            'C2 H3 F10 N Sb2'
_chemical_formula_weight         474.55

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.0562 5.8946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.7664(5)
_cell_length_b                   8.2163(4)
_cell_length_c                   8.6861(5)
_cell_angle_alpha                90.605(4)
_cell_angle_beta                 114.993(6)
_cell_angle_gamma                91.614(4)
_cell_volume                     502.01(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    1078
_cell_measurement_theta_min      17.2480
_cell_measurement_theta_max      65.5670

_exptl_crystal_description       'truncated prism'
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.139
_exptl_crystal_F_000             428
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.046

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 1 -5 0.0484
-2 4 3 0.0254
2 -5 -2 0.0180
1 -5 -3 0.0181
-5 -1 3 0.0218
-1 2 -4 0.0489
4 -2 -5 0.0221
1 -4 3 0.0638
2 -1 -5 0.0301
-1 -1 5 0.0614
5 1 -3 0.0348
-2 5 1 0.0377
-1 1 5 0.0535

_exptl_absorpt_coefficient_mu    43.957
_shelx_estimated_absorpt_T_min   0.073
_shelx_estimated_absorpt_T_max   0.237
_exptl_absorpt_correction_T_min  0.061
_exptl_absorpt_correction_T_max  0.339
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
_diffrn_detector_area_resol_mean 5.2548
_diffrn_measurement_method       'ω scans'

_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.4779 2781 794 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000
1.0000
2 0.5221 2836 794 nmt -0.9999 -0.0524 -0.0000 -0.0003 1.0002 -0.0002 0.0000
-0.0229 -1.0002
_oxdiff_twin_integration_method  simultaneous
_twin_special_details            
;
Component 2 rotated by -179.9979° 
 around [-0.03 1.00 -0.01] (reciprocal) or [-0.00 1.00 0.00] (direct)
;

_diffrn_reflns_number            3077
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_av_R_equivalents  0.0993
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         5.388
_diffrn_reflns_theta_max         66.034
_diffrn_reflns_theta_full        66.034
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             3077
_reflns_number_gt                2414
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    SHELXT
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
'Refined as a 2-component perfect twin from HKLF 5 data.,Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1705P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3077
_refine_ls_number_parameters     137
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0772
_refine_ls_wR_factor_ref         0.2117
_refine_ls_wR_factor_gt          0.2062
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb 0.34786(11) 0.25275(11) 0.57271(10) 0.0236(4) Uani 1 1 d . . . . .
Sb2 Sb 0.12410(11) 0.25270(10) 0.90603(10) 0.0218(4) Uani 1 1 d . . . . .
F1 F 0.2724(15) 0.3034(14) 0.7622(12) 0.044(2) Uani 1 1 d . . . . .
F2 F 0.3073(14) 0.0380(11) 0.6093(13) 0.042(2) Uani 1 1 d . . . . .
F3 F 0.3945(14) 0.2111(14) 0.3861(13) 0.047(2) Uani 1 1 d . . . . .
F4 F 0.3436(13) 0.4756(10) 0.5517(13) 0.035(2) Uani 1 1 d . . . . .
F5 F 0.5947(13) 0.2563(14) 0.7322(13) 0.048(2) Uani 1 1 d . . . . .
F6 F -0.0180(14) 0.1085(12) 0.7283(11) 0.039(2) Uani 1 1 d . . . . .
F7 F 0.3013(13) 0.0933(11) 0.9998(13) 0.037(2) Uani 1 1 d . . . . .
F8 F 0.2976(13) 0.4045(11) 1.0547(12) 0.034(2) Uani 1 1 d . . . . .
F9 F -0.0209(14) 0.4242(12) 0.7886(13) 0.045(2) Uani 1 1 d . . . . .
F10 F -0.0061(13) 0.2116(12) 1.0354(11) 0.037(2) Uani 1 1 d . . . . .
N1 N 0.0589(16) 0.2530(15) 0.4192(16) 0.027(2) Uani 1 1 d . . . . .
C1 C -0.095(2) 0.2563(16) 0.3180(19) 0.025(3) Uani 1 1 d . . . . .
C2 C -0.2873(18) 0.2590(18) 0.195(2) 0.027(3) Uani 1 1 d . . . . .
H2A H -0.321678 0.156161 0.128976 0.040 Uiso 1 1 calc R U . . .
H2B H -0.301910 0.349673 0.118451 0.040 Uiso 1 1 calc R U . . .
H2C H -0.370686 0.272942 0.252519 0.040 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sb1 0.0154(6) 0.0388(7) 0.0176(6) -0.0007(4) 0.0082(4) -0.0016(4)
Sb2 0.0165(5) 0.0342(6) 0.0158(6) -0.0004(4) 0.0082(4) -0.0025(4)
F1 0.041(5) 0.063(6) 0.033(5) -0.013(4) 0.023(5) -0.022(4)
F2 0.032(5) 0.039(5) 0.041(6) 0.003(4) 0.002(5) 0.003(4)
F3 0.032(5) 0.079(7) 0.041(6) -0.008(5) 0.028(5) -0.004(5)
F4 0.027(5) 0.037(5) 0.041(5) -0.002(4) 0.015(4) -0.006(4)
F5 0.018(4) 0.074(7) 0.039(5) -0.004(5) -0.001(4) 0.001(4)
F6 0.032(5) 0.056(6) 0.021(5) -0.012(4) 0.005(4) -0.016(4)
F7 0.030(5) 0.040(5) 0.038(5) 0.004(4) 0.011(4) 0.009(4)
F8 0.029(5) 0.043(5) 0.027(5) -0.007(4) 0.011(4) -0.003(4)
F9 0.030(5) 0.051(6) 0.041(6) 0.017(5) 0.003(5) 0.010(4)
F10 0.029(4) 0.056(6) 0.033(5) -0.001(4) 0.020(4) 0.002(4)
N1 0.009(6) 0.037(6) 0.031(6) -0.005(5) 0.007(5) -0.003(4)
C1 0.027(8) 0.023(7) 0.037(8) 0.000(6) 0.025(8) -0.004(5)
C2 0.012(6) 0.043(8) 0.026(7) -0.004(6) 0.010(6) -0.003(6)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sb1 F5 1.830(9) . ?
Sb1 F3 1.835(9) . ?
Sb1 F2 1.838(9) . ?
Sb1 F4 1.841(9) . ?
Sb1 F1 2.010(8) . ?
Sb1 N1 2.070(12) . ?
Sb2 F10 1.830(7) . ?
Sb2 F8 1.855(9) . ?
Sb2 F9 1.855(9) . ?
Sb2 F7 1.857(9) . ?
Sb2 F6 1.858(9) . ?
Sb2 F1 2.064(8) . ?
N1 C1 1.15(2) . ?
C1 C2 1.43(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F5 Sb1 F3 97.5(5) . . ?
F5 Sb1 F2 92.8(5) . . ?
F3 Sb1 F2 95.2(5) . . ?
F5 Sb1 F4 93.8(5) . . ?
F3 Sb1 F4 95.5(5) . . ?
F2 Sb1 F4 166.6(5) . . ?
F5 Sb1 F1 87.7(4) . . ?
F3 Sb1 F1 174.7(4) . . ?
F2 Sb1 F1 85.7(5) . . ?
F4 Sb1 F1 82.9(4) . . ?
F5 Sb1 N1 172.3(5) . . ?
F3 Sb1 N1 90.2(5) . . ?
F2 Sb1 N1 86.0(5) . . ?
F4 Sb1 N1 85.9(5) . . ?
F1 Sb1 N1 84.7(4) . . ?
F10 Sb2 F8 96.5(4) . . ?
F10 Sb2 F9 96.3(4) . . ?
F8 Sb2 F9 88.4(4) . . ?
F10 Sb2 F7 95.8(4) . . ?
F8 Sb2 F7 88.9(4) . . ?
F9 Sb2 F7 167.7(4) . . ?
F10 Sb2 F6 96.6(4) . . ?
F8 Sb2 F6 166.9(4) . . ?
F9 Sb2 F6 90.7(5) . . ?
F7 Sb2 F6 89.2(4) . . ?
F10 Sb2 F1 178.9(4) . . ?
F8 Sb2 F1 82.6(4) . . ?
F9 Sb2 F1 83.2(4) . . ?
F7 Sb2 F1 84.6(4) . . ?
F6 Sb2 F1 84.4(4) . . ?
Sb1 F1 Sb2 152.4(6) . . ?
C1 N1 Sb1 171.5(11) . . ?
N1 C1 C2 178.7(14) . . ?

_refine_diff_density_max         1.768
_refine_diff_density_min         -2.310
_refine_diff_density_rms         0.384

_shelx_res_file                  
;
TITL ayt88 in P-1 at 123K Gemini-Cu twin 75% of profile
    88.res
    created by SHELXL-2018/3 at 12:39:29 on 11-Sep-2019
CELL 1.54184 7.766377 8.216302 8.686114 90.6049 114.9932 91.6137
ZERR 2 0.000466   0.000383   0.000534   0.0044   0.0060   0.0043
LATT 1
SFAC C H N  F Sb
UNIT 4 6 2 20 4

TEMP -150
rem _diffrn_reflns_av_R_equivalents 0.0993
L.S. 10
MERG 0
PLAN  10
SIZE 0.125 0.074 0.046
fmap 2
acta 135

WGHT    0.170500
FVAR       4.89781
SB1   5    0.347861    0.252754    0.572713    11.00000    0.01538    0.03881 =
         0.01758   -0.00065    0.00822   -0.00157
SB2   5    0.124095    0.252704    0.906027    11.00000    0.01651    0.03417 =
         0.01582   -0.00043    0.00820   -0.00247
F1    4    0.272442    0.303412    0.762197    11.00000    0.04118    0.06336 =
         0.03251   -0.01289    0.02339   -0.02167
F2    4    0.307265    0.037979    0.609280    11.00000    0.03183    0.03867 =
         0.04100    0.00342    0.00238    0.00316
F3    4    0.394478    0.211100    0.386056    11.00000    0.03197    0.07862 =
         0.04125   -0.00797    0.02756   -0.00407
F4    4    0.343616    0.475553    0.551676    11.00000    0.02726    0.03678 =
         0.04149   -0.00237    0.01505   -0.00601
F5    4    0.594724    0.256267    0.732239    11.00000    0.01757    0.07429 =
         0.03929   -0.00449   -0.00144    0.00067
F6    4   -0.017969    0.108496    0.728275    11.00000    0.03169    0.05632 =
         0.02064   -0.01174    0.00517   -0.01612
F7    4    0.301310    0.093295    0.999786    11.00000    0.02955    0.04023 =
         0.03826    0.00372    0.01141    0.00893
F8    4    0.297559    0.404526    1.054702    11.00000    0.02917    0.04337 =
         0.02734   -0.00655    0.01098   -0.00275
F9    4   -0.020928    0.424162    0.788557    11.00000    0.03036    0.05109 =
         0.04077    0.01706    0.00300    0.01000
F10   4   -0.006130    0.211646    1.035394    11.00000    0.02861    0.05634 =
         0.03258   -0.00132    0.02025    0.00225
N1    3    0.058918    0.252991    0.419207    11.00000    0.00899    0.03715 =
         0.03135   -0.00450    0.00676   -0.00289
C1    1   -0.094775    0.256266    0.317986    11.00000    0.02695    0.02293 =
         0.03673    0.00044    0.02547   -0.00378
C2    1   -0.287295    0.258972    0.194870    11.00000    0.01196    0.04322 =
         0.02632   -0.00444    0.01018   -0.00306
AFIX 137
H2A   2   -0.321678    0.156161    0.128976    11.00000   -1.50000
H2B   2   -0.301910    0.349673    0.118451    11.00000   -1.50000
H2C   2   -0.370686    0.272942    0.252519    11.00000   -1.50000
AFIX   0
HKLF 5




REM  ayt88 in P-1 at 123K Gemini-Cu twin 75% of profile
REM wR2 = 0.2117, GooF = S = 1.008, Restrained GooF = 1.008 for all data
REM R1 = 0.0772 for 2414 Fo > 4sig(Fo) and 0.0854 for all 3077 data
REM 137 parameters refined using 0 restraints

END

WGHT      0.1703      0.0000

REM Highest difference peak  1.768,  deepest hole -2.310,  1-sigma level  0.384
Q1    1   0.0479  0.1657  0.8347  11.00000  0.05    1.77
Q2    1   0.2387  0.1391  0.5247  11.00000  0.05    1.68
Q3    1   0.3825  0.3438  0.7450  11.00000  0.05    1.68
Q4    1   0.2538  0.3695  0.9545  11.00000  0.05    1.66
Q5    1   0.0003  0.1435  0.8725  11.00000  0.05    1.64
Q6    1   0.0845  0.1660  0.7407  11.00000  0.05    1.60
Q7    1   0.1950  0.2592  0.8134  11.00000  0.05    1.57
Q8    1   0.4660  0.3650  0.6206  11.00000  0.05    1.56
Q9    1   0.1731  0.3469  1.0836  11.00000  0.05    1.51
Q10   1   0.3133  0.1462  0.4066  11.00000  0.05    1.50
;
_shelx_res_checksum              76605

_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_3ayt86
_database_code_depnum_ccdc_archive 'CCDC 2086687'
loop_
_audit_author_name
_audit_author_address
'Alexander Virovets'
;University of Regensburg
Germany
;
_audit_update_record             
;
2021-05-29 deposited with the CCDC.	2021-08-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT972_3ayt86              
;
PROBLEM: Check Calcd Resid. Dens.  1.00A   From Sb2            -2.64 eA-3  
RESPONSE: The reason is huge X-ray absorbtion from plate shaped crystal.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H10 F12 N2 Sb4'
_chemical_formula_weight         873.20

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.0562 5.8946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   11.7020(3)
_cell_length_b                   5.64449(17)
_cell_length_c                   14.5489(5)
_cell_angle_alpha                90
_cell_angle_beta                 101.913(3)
_cell_angle_gamma                90
_cell_volume                     940.29(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    2462
_cell_measurement_theta_min      3.8340
_cell_measurement_theta_max      65.7480

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.084
_exptl_crystal_F_000             792
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.191
_exptl_crystal_size_mid          0.161
_exptl_crystal_size_min          0.022

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
5 0 3 0.0237
3 2 -5 0.0876
-3 -2 5 0.0996
-5 0 8 0.1057
4 -2 -5 0.0763
-5 0 -3 0.0010
1 0 -1 0.0852
-1 2 1 0.0913
1 -2 -1 0.0913
-4 2 5 0.1033

_exptl_absorpt_coefficient_mu    46.205
_shelx_estimated_absorpt_T_min   0.041
_shelx_estimated_absorpt_T_max   0.430
_exptl_absorpt_correction_T_min  0.022
_exptl_absorpt_correction_T_max  0.373
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.21a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
_diffrn_detector_area_resol_mean 5.2548
_diffrn_reflns_number            4097
_diffrn_reflns_av_unetI/netI     0.0585
_diffrn_reflns_av_R_equivalents  0.0773
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.860
_diffrn_reflns_theta_max         65.954
_diffrn_reflns_theta_full        65.954
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             1636
_reflns_number_gt                1370
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_computing_structure_solution    SHELXT
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1029P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1636
_refine_ls_number_parameters     127
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0541
_refine_ls_wR_factor_ref         0.1378
_refine_ls_wR_factor_gt          0.1344
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb 0.32990(5) 0.55303(10) 0.41771(4) 0.0132(3) Uani 1 1 d . . . . .
Sb2 Sb 0.58392(4) 0.96816(11) 0.36513(4) 0.0130(3) Uani 1 1 d . . . . .
F1 F 0.3018(4) 0.6766(10) 0.5350(3) 0.0168(11) Uani 1 1 d . . . . .
F2 F 0.2854(5) 0.8530(11) 0.3588(4) 0.0217(12) Uani 1 1 d . . . . .
F3 F 0.4850(4) 0.7309(11) 0.4652(4) 0.0224(12) Uani 1 1 d . . . . .
F4 F 0.5455(5) 0.6699(12) 0.2986(4) 0.0291(14) Uani 1 1 d . . . . .
F5 F 0.7063(4) 0.8188(10) 0.4547(3) 0.0165(11) Uani 1 1 d . . . . .
F6 F 0.7013(5) 1.0086(12) 0.2887(4) 0.0247(13) Uani 1 1 d . . . . .
N1 N 0.1268(7) 0.5185(15) 0.3936(6) 0.0147(16) Uani 1 1 d . . . . .
C1 C 0.0748(8) 0.3223(19) 0.3519(6) 0.018(2) Uani 1 1 d . . . . .
H1 H 0.121602 0.196124 0.337072 0.022 Uiso 1 1 calc R U . . .
C2 C -0.0450(8) 0.301(2) 0.3304(7) 0.022(2) Uani 1 1 d . . . . .
H2 H -0.080488 0.160887 0.301436 0.027 Uiso 1 1 calc R U . . .
C3 C -0.1132(8) 0.485(2) 0.3511(7) 0.024(2) Uani 1 1 d . . . . .
H3 H -0.195950 0.475075 0.335079 0.029 Uiso 1 1 calc R U . . .
C4 C -0.0589(8) 0.685(2) 0.3959(7) 0.021(2) Uani 1 1 d . . . . .
H4 H -0.103567 0.811901 0.412913 0.025 Uiso 1 1 calc R U . . .
C5 C 0.0602(8) 0.6947(19) 0.4148(6) 0.0181(19) Uani 1 1 d . . . . .
H5 H 0.097446 0.832576 0.444223 0.022 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sb1 0.0137(4) 0.0135(5) 0.0150(4) 0.0000(2) 0.0093(2) -0.00003(19)
Sb2 0.0134(4) 0.0134(4) 0.0147(4) 0.0003(2) 0.0084(2) -0.00100(19)
F1 0.020(2) 0.017(3) 0.015(2) -0.003(2) 0.009(2) -0.002(2)
F2 0.024(2) 0.020(3) 0.023(3) 0.005(3) 0.011(2) 0.001(2)
F3 0.014(2) 0.024(3) 0.033(3) 0.000(3) 0.012(2) -0.003(2)
F4 0.033(3) 0.030(4) 0.025(3) -0.004(3) 0.009(2) -0.004(3)
F5 0.019(2) 0.014(3) 0.018(3) 0.005(2) 0.007(2) 0.004(2)
F6 0.023(3) 0.033(3) 0.022(3) 0.001(3) 0.012(2) -0.001(3)
N1 0.020(4) 0.011(4) 0.019(4) -0.002(3) 0.017(3) -0.004(3)
C1 0.032(5) 0.013(5) 0.012(4) -0.001(4) 0.011(4) -0.005(4)
C2 0.026(4) 0.020(5) 0.023(5) -0.002(5) 0.011(4) -0.009(4)
C3 0.017(4) 0.042(7) 0.016(5) 0.010(5) 0.010(4) -0.006(4)
C4 0.022(4) 0.021(6) 0.024(5) 0.009(4) 0.017(4) 0.003(4)
C5 0.023(4) 0.019(5) 0.015(4) -0.002(4) 0.012(3) 0.004(4)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sb1 F2 1.921(6) . ?
Sb1 F1 1.933(5) . ?
Sb1 F3 2.065(5) . ?
Sb1 N1 2.338(8) . ?
Sb2 F5 1.920(5) . ?
Sb2 F4 1.948(6) . ?
Sb2 F6 1.951(6) . ?
Sb2 F3 2.438(5) . ?
Sb2 F1 2.668(5) 3_676 ?
N1 C5 1.338(13) . ?
N1 C1 1.346(13) . ?
C1 C2 1.377(13) . ?
C1 H1 0.9500 . ?
C2 C3 1.380(16) . ?
C2 H2 0.9500 . ?
C3 C4 1.390(16) . ?
C3 H3 0.9500 . ?
C4 C5 1.364(14) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F2 Sb1 F1 89.8(2) . . ?
F2 Sb1 F3 81.9(2) . . ?
F1 Sb1 F3 80.1(2) . . ?
F2 Sb1 N1 80.4(3) . . ?
F1 Sb1 N1 79.0(2) . . ?
F3 Sb1 N1 152.5(3) . . ?
F5 Sb2 F4 91.2(2) . . ?
F5 Sb2 F6 85.6(2) . . ?
F4 Sb2 F6 86.3(3) . . ?
F5 Sb2 F3 74.52(19) . . ?
F4 Sb2 F3 74.5(2) . . ?
F6 Sb2 F3 151.8(2) . . ?
F5 Sb2 F1 75.0(2) . 3_676 ?
F4 Sb2 F1 163.4(2) . 3_676 ?
F6 Sb2 F1 83.7(2) . 3_676 ?
F3 Sb2 F1 109.51(17) . 3_676 ?
Sb1 F1 Sb2 126.5(2) . 3_676 ?
Sb1 F3 Sb2 124.1(3) . . ?
C5 N1 C1 119.0(8) . . ?
C5 N1 Sb1 121.7(6) . . ?
C1 N1 Sb1 119.2(6) . . ?
N1 C1 C2 121.2(10) . . ?
N1 C1 H1 119.4 . . ?
C2 C1 H1 119.4 . . ?
C1 C2 C3 119.4(10) . . ?
C1 C2 H2 120.3 . . ?
C3 C2 H2 120.3 . . ?
C2 C3 C4 119.0(9) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C5 C4 C3 118.5(10) . . ?
C5 C4 H4 120.8 . . ?
C3 C4 H4 120.8 . . ?
N1 C5 C4 122.9(10) . . ?
N1 C5 H5 118.6 . . ?
C4 C5 H5 118.6 . . ?

_refine_diff_density_max         2.145
_refine_diff_density_min         -2.636
_refine_diff_density_rms         0.446

_shelx_res_file                  
;
TITL ayt86 in P2(1)/c at 123K Gemini-Cu noerr
    86.res
    created by SHELXL-2018/3 at 11:31:17 on 11-Sep-2019
CELL 1.54178  11.70202   5.64449  14.54889  90.0000 101.9126  90.0000
ZERR    2.00   0.00033   0.00017   0.00046   0.0000   0.0029   0.0000
LATT  1
SYMM -X, 0.5+Y, 0.5-Z
SFAC C H N F SB
UNIT 20 20 4 24 8

L.S. 10
PLAN  10
SIZE 0.191 0.161 0.022
TEMP -150
CONN 12 1.6 $Sb
BOND $H
FMAP 2
ACTA 135

WGHT    0.102900
FVAR       0.08083
SB1   5    0.329904    0.553026    0.417712    11.00000    0.01368    0.01354 =
         0.01501    0.00002    0.00932   -0.00003
SB2   5    0.583915    0.968157    0.365126    11.00000    0.01342    0.01338 =
         0.01471    0.00031    0.00839   -0.00100
F1    4    0.301802    0.676635    0.534995    11.00000    0.02016    0.01749 =
         0.01515   -0.00276    0.00903   -0.00221
F2    4    0.285427    0.853029    0.358760    11.00000    0.02397    0.02046 =
         0.02315    0.00519    0.01057    0.00114
F3    4    0.485043    0.730854    0.465156    11.00000    0.01412    0.02364 =
         0.03262    0.00006    0.01225   -0.00305
F4    4    0.545514    0.669854    0.298592    11.00000    0.03340    0.02966 =
         0.02538   -0.00415    0.00898   -0.00447
F5    4    0.706265    0.818827    0.454686    11.00000    0.01884    0.01422 =
         0.01778    0.00470    0.00718    0.00390
F6    4    0.701346    1.008580    0.288730    11.00000    0.02307    0.03252 =
         0.02178    0.00123    0.01208   -0.00056
N1    3    0.126789    0.518474    0.393623    11.00000    0.01979    0.01104 =
         0.01896   -0.00175    0.01703   -0.00369
C1    1    0.074784    0.322258    0.351912    11.00000    0.03205    0.01270 =
         0.01224   -0.00146    0.01146   -0.00526
AFIX  43
H1    2    0.121602    0.196124    0.337072    11.00000   -1.20000
AFIX   0
C2    1   -0.045043    0.301000    0.330356    11.00000    0.02606    0.02031 =
         0.02334   -0.00231    0.01118   -0.00910
AFIX  43
H2    2   -0.080488    0.160887    0.301436    11.00000   -1.20000
AFIX   0
C3    1   -0.113177    0.484985    0.351128    11.00000    0.01654    0.04230 =
         0.01642    0.01037    0.01018   -0.00589
AFIX  43
H3    2   -0.195950    0.475075    0.335079    11.00000   -1.20000
AFIX   0
C4    1   -0.058850    0.684928    0.395873    11.00000    0.02158    0.02105 =
         0.02423    0.00928    0.01714    0.00314
AFIX  43
H4    2   -0.103567    0.811901    0.412913    11.00000   -1.20000
AFIX   0
C5    1    0.060204    0.694659    0.414766    11.00000    0.02349    0.01922 =
         0.01513   -0.00155    0.01236    0.00352
AFIX  43
H5    2    0.097446    0.832576    0.444223    11.00000   -1.20000

AFIX   0
HKLF 4




REM  ayt86 in P2(1)/c at 123K Gemini-Cu noerr
REM wR2 = 0.1378, GooF = S = 1.012, Restrained GooF = 1.012 for all data
REM R1 = 0.0541 for 1370 Fo > 4sig(Fo) and 0.0606 for all 1636 data
REM 127 parameters refined using 0 restraints

END

WGHT      0.1028      0.0000

REM Highest difference peak  2.145,  deepest hole -2.636,  1-sigma level  0.446
Q1    1   0.4095  0.4557  0.4165  11.00000  0.05    2.15
Q2    1   0.6970  0.9097  0.3591  11.00000  0.05    1.55
Q3    1   0.1451  1.0452  0.4944  11.00000  0.05    1.55
Q4    1   0.3597  0.9836  0.3183  11.00000  0.05    1.43
Q5    1   0.3962  0.8576  0.3538  11.00000  0.05    1.42
Q6    1  -0.3202  0.5189  0.2839  11.00000  0.05    1.40
Q7    1   0.3167  0.4162  0.4642  11.00000  0.05    1.38
Q8    1   0.5951  0.7166  0.4347  11.00000  0.05    1.38
Q9    1   0.3459  0.7982  0.4956  11.00000  0.05    1.27
Q10   1   0.7796  0.9648  0.5253  11.00000  0.05    1.25
;
_shelx_res_checksum              9731

_chemical_properties_physical    Air-sensitive,Moisture-sensitive
