# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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_Me3As_150K
_database_code_depnum_ccdc_archive 'CCDC 2057063'
_audit_update_record             
;
2021-01-18 deposited with the CCDC.	2021-12-01 downloaded from the CCDC.
;

# CHEMICAL DATA

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H9 As'
_chemical_formula_sum            'C3 H9 As'
_chemical_formula_weight         120.02

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'

# CRYSTAL DATA

_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_H-M_alt        'C m c 21'
_space_group_name_Hall           'C 2c -2'

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

_cell_length_a                   9.3417(7)
_cell_length_b                   10.9779(7)
_cell_length_c                   5.2141(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     534.72(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.0(1)
_cell_measurement_reflns_used    3032
_cell_measurement_theta_min      2.87
_cell_measurement_theta_max      30.93

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_F_000             240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    6.179
_shelx_estimated_absorpt_T_min   0.37
_shelx_estimated_absorpt_T_max   0.58
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.02
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?


# EXPERIMENTAL DATA

_exptl_special_details           
; 
Data were collected for the in-situ low-temperature crystallized
single crystal. 
;
_diffrn_ambient_temperature      150.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 8.0951
_diffrn_reflns_number            4078
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         2.863
_diffrn_reflns_theta_max         25.894
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             554
_reflns_number_gt                546
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.788
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_cell_refinement       
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_data_reduction        
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury (Macrae at al., 2020)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

# REFINEMENT DATA 

_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1011P)²+0.2613P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.09(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         554
_refine_ls_number_parameters     29
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0481
_refine_ls_wR_factor_ref         0.1227
_refine_ls_wR_factor_gt          0.1223
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.093
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.5000 0.29523(6) 0.35569(2) 0.0339(5) Uani 1 2 d DS T P . .
C1 C 0.3438(10) 0.3667(8) 0.1546(18) 0.045(2) Uani 1 1 d . . . . .
H11 H 0.3615 0.3537 -0.0247 0.067 Uiso 1 1 calc R U . . .
H12 H 0.3383 0.4525 0.1884 0.067 Uiso 1 1 calc R U . . .
H13 H 0.2550 0.3287 0.2015 0.067 Uiso 1 1 calc R U . . .
C2 C 0.5000 0.1360(3) 0.1860(6) 0.047(3) Uani 1 2 d DS T P . .
H21 H 0.5000 0.1472(2) 0.0033(4) 0.071 Uiso 1 2 d DS U P . .
H22 H 0.58392(2) 0.09132(10) 0.2357(6) 0.071 Uiso 1 1 d D U . . .


# MOLECULAR GEOMETRY

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As1 C2 1.960(3) . ?
As1 C1 1.961(9) . ?
As1 C1 1.961(9) 3_655 ?
C1 H11 0.9600 . ?
C1 H12 0.9600 . ?
C1 H13 0.9600 . ?
C2 H21 0.9601(14) . ?
C2 H22 0.9602(14) . ?

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
C2 As1 C1 96.6(3) . . ?
C2 As1 C1 96.6(3) . 3_655 ?
C1 As1 C1 96.2(6) . 3_655 ?
As1 C1 H11 109.5 . . ?
As1 C1 H12 109.5 . . ?
H11 C1 H12 109.5 . . ?
As1 C1 H13 109.5 . . ?
H11 C1 H13 109.5 . . ?
H12 C1 H13 109.5 . . ?
As1 C2 H21 109.5(2) . . ?
As1 C2 H22 109.47(16) . . ?
H21 C2 H22 109.47(16) . . ?

_refine_diff_density_max         0.277
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.083


####################################################################### 
# 
# 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_Me3Sb_C6F5I_100K
_database_code_depnum_ccdc_archive 'CCDC 2057076'
_audit_update_record             
;
2021-01-18 deposited with the CCDC.	2021-12-01 downloaded from the CCDC.
;

# CHEMICAL DATA

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H9 Sb, C6 F5 I'
_chemical_formula_sum            'C9 H9 F5 I Sb'
_chemical_formula_weight         460.82

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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

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

_cell_length_a                   19.9342(16)
_cell_length_b                   5.9935(3)
_cell_length_c                   23.6586(14)
_cell_angle_alpha                90
_cell_angle_beta                 109.451(7)
_cell_angle_gamma                90
_cell_volume                     2665.3(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    100.0(1)
_cell_measurement_reflns_used    9486
_cell_measurement_theta_min      2.07
_cell_measurement_theta_max      31.96

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.297
_exptl_crystal_F_000             1696
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    4.417
_shelx_estimated_absorpt_T_min   0.67
_shelx_estimated_absorpt_T_max   0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.28
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?


# EXPERIMENTAL DATA

_exptl_special_details           
; 
Data were collected for the in-situ low-temperature cocrystallized
single crystal. 
;
_diffrn_ambient_temperature      100.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 8.0951
_diffrn_reflns_number            16495
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.167
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2627
_reflns_number_gt                2394
_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 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_cell_refinement       
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_data_reduction        
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury (Macrae at al., 2020)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

# REFINEMENT DATA 

_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)+(0.0254P)²+7.6501P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2627
_refine_ls_number_parameters     148
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0275
_refine_ls_wR_factor_ref         0.0629
_refine_ls_wR_factor_gt          0.0613
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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 0.27152(2) 0.39950(5) 0.39491(2) 0.02730(10) Uani 1 1 d . . . . .
C1 C 0.1802(3) 0.1924(9) 0.3790(3) 0.0571(16) Uani 1 1 d . . . . .
H11 H 0.1657 0.1372 0.3386 0.086 Uiso 1 1 calc R U . . .
H12 H 0.1422 0.2776 0.3847 0.086 Uiso 1 1 calc R U . . .
H13 H 0.1916 0.0692 0.4065 0.086 Uiso 1 1 calc R U . . .
C2 C 0.3310(3) 0.1660(8) 0.3618(2) 0.0381(11) Uani 1 1 d . . . . .
H21 H 0.3682 0.2431 0.3525 0.057 Uiso 1 1 calc R U . . .
H22 H 0.3000 0.0954 0.3263 0.057 Uiso 1 1 calc R U . . .
H23 H 0.3515 0.0549 0.3918 0.057 Uiso 1 1 calc R U . . .
C3 C 0.2304(3) 0.5820(9) 0.3136(2) 0.0521(15) Uani 1 1 d . . . . .
H31 H 0.2101 0.4804 0.2810 0.078 Uiso 1 1 calc R U . . .
H32 H 0.2681 0.6648 0.3066 0.078 Uiso 1 1 calc R U . . .
H33 H 0.1943 0.6833 0.3164 0.078 Uiso 1 1 calc R U . . .
I1 I 0.37490(2) 0.72881(4) 0.51402(2) 0.02433(9) Uani 1 1 d . . . . .
C4 C 0.4474(2) 0.9250(6) 0.57978(17) 0.0207(8) Uani 1 1 d . . . . .
F1 F 0.44759(14) 0.6692(4) 0.65585(10) 0.0319(6) Uani 1 1 d . . . . .
C5 C 0.4706(2) 0.8624(6) 0.63939(17) 0.0239(9) Uani 1 1 d . . . . .
F2 F 0.53931(15) 0.9230(4) 0.74032(10) 0.0383(7) Uani 1 1 d . . . . .
C6 C 0.5165(2) 0.9917(7) 0.68291(17) 0.0281(10) Uani 1 1 d . . . . .
F3 F 0.58525(14) 1.3189(4) 0.70945(11) 0.0370(6) Uani 1 1 d . . . . .
C7 C 0.5403(2) 1.1909(7) 0.66765(19) 0.0274(9) Uani 1 1 d . . . . .
F4 F 0.54249(14) 1.4506(4) 0.59398(11) 0.0334(6) Uani 1 1 d . . . . .
C8 C 0.5183(2) 1.2572(6) 0.60827(19) 0.0251(9) Uani 1 1 d . . . . .
F5 F 0.45256(14) 1.1925(4) 0.50820(10) 0.0288(5) Uani 1 1 d . . . . .
C9 C 0.4728(2) 1.1241(6) 0.56530(17) 0.0216(8) Uani 1 1 d . . . . .


# MOLECULAR GEOMETRY

_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 C3 2.126(5) . ?
Sb1 C1 2.130(5) . ?
Sb1 C2 2.145(5) . ?
C1 H11 0.9600 . ?
C1 H12 0.9600 . ?
C1 H13 0.9600 . ?
C2 H21 0.9600 . ?
C2 H22 0.9600 . ?
C2 H23 0.9600 . ?
C3 H31 0.9600 . ?
C3 H32 0.9600 . ?
C3 H33 0.9600 . ?
I1 C4 2.097(4) . ?
C4 C5 1.382(5) . ?
C4 C9 1.382(6) . ?
F1 C5 1.350(5) . ?
C5 C6 1.367(6) . ?
F2 C6 1.345(4) . ?
C6 C7 1.377(6) . ?
F3 C7 1.334(5) . ?
C7 C8 1.383(6) . ?
F4 C8 1.341(5) . ?
C8 C9 1.371(6) . ?
F5 C9 1.339(4) . ?

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
C3 Sb1 C1 95.2(2) . . ?
C3 Sb1 C2 95.7(2) . . ?
C1 Sb1 C2 95.7(2) . . ?
Sb1 C1 H11 109.5 . . ?
Sb1 C1 H12 109.5 . . ?
H11 C1 H12 109.5 . . ?
Sb1 C1 H13 109.5 . . ?
H11 C1 H13 109.5 . . ?
H12 C1 H13 109.5 . . ?
Sb1 C2 H21 109.5 . . ?
Sb1 C2 H22 109.5 . . ?
H21 C2 H22 109.5 . . ?
Sb1 C2 H23 109.5 . . ?
H21 C2 H23 109.5 . . ?
H22 C2 H23 109.5 . . ?
Sb1 C3 H31 109.5 . . ?
Sb1 C3 H32 109.5 . . ?
H31 C3 H32 109.5 . . ?
Sb1 C3 H33 109.5 . . ?
H31 C3 H33 109.5 . . ?
H32 C3 H33 109.5 . . ?
C5 C4 C9 117.5(4) . . ?
C5 C4 I1 121.2(3) . . ?
C9 C4 I1 121.2(3) . . ?
F1 C5 C6 118.4(3) . . ?
F1 C5 C4 119.8(4) . . ?
C6 C5 C4 121.8(4) . . ?
F2 C6 C5 120.2(4) . . ?
F2 C6 C7 120.0(4) . . ?
C5 C6 C7 119.8(4) . . ?
F3 C7 C6 120.6(4) . . ?
F3 C7 C8 119.7(4) . . ?
C6 C7 C8 119.7(4) . . ?
F4 C8 C9 121.4(4) . . ?
F4 C8 C7 119.0(4) . . ?
C9 C8 C7 119.6(4) . . ?
F5 C9 C8 118.2(4) . . ?
F5 C9 C4 120.2(3) . . ?
C8 C9 C4 121.7(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 C4 C5 F1 -179.8(4) . . . . ?
I1 C4 C5 F1 1.5(5) . . . . ?
C9 C4 C5 C6 0.4(6) . . . . ?
I1 C4 C5 C6 -178.3(3) . . . . ?
F1 C5 C6 F2 1.9(6) . . . . ?
C4 C5 C6 F2 -178.4(4) . . . . ?
F1 C5 C6 C7 -179.3(4) . . . . ?
C4 C5 C6 C7 0.5(7) . . . . ?
F2 C6 C7 F3 -0.9(6) . . . . ?
C5 C6 C7 F3 -179.8(4) . . . . ?
F2 C6 C7 C8 178.0(4) . . . . ?
C5 C6 C7 C8 -0.8(7) . . . . ?
F3 C7 C8 F4 -0.4(6) . . . . ?
C6 C7 C8 F4 -179.4(4) . . . . ?
F3 C7 C8 C9 179.3(4) . . . . ?
C6 C7 C8 C9 0.3(6) . . . . ?
F4 C8 C9 F5 -0.2(6) . . . . ?
C7 C8 C9 F5 -179.9(4) . . . . ?
F4 C8 C9 C4 -179.7(4) . . . . ?
C7 C8 C9 C4 0.6(6) . . . . ?
C5 C4 C9 F5 179.5(4) . . . . ?
I1 C4 C9 F5 -1.8(5) . . . . ?
C5 C4 C9 C8 -1.0(6) . . . . ?
I1 C4 C9 C8 177.7(3) . . . . ?

_refine_diff_density_max         0.943
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.125



#############################################################################


####################################################################### 
# 
# 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_Me3As_C6F5I_220K
_database_code_depnum_ccdc_archive 'CCDC 2057069'
_audit_update_record             
;
2021-01-18 deposited with the CCDC.	2021-12-01 downloaded from the CCDC.
;

# CHEMICAL DATA

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H9 As, C6 F5 I'
_chemical_formula_sum            'C9 H9 As F5 I'
_chemical_formula_weight         413.98

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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_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                   11.5901(3)
_cell_length_b                   11.6731(3)
_cell_length_c                   20.0896(5)
_cell_angle_alpha                90
_cell_angle_beta                 102.821(3)
_cell_angle_gamma                90
_cell_volume                     2650.21(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    220.0(1)
_cell_measurement_reflns_used    7506
_cell_measurement_theta_min      2.08
_cell_measurement_theta_max      25.36

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.075
_exptl_crystal_F_000             1552
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    4.925
_shelx_estimated_absorpt_T_min   0.32
_shelx_estimated_absorpt_T_max   0.44
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.04
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?


# EXPERIMENTAL DATA

_exptl_special_details           
; 
Data were collected for the in-situ low-temperature cocrystallized
single crystal. 
;
_diffrn_ambient_temperature      220.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 8.0951
_diffrn_reflns_number            18349
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.079
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2603
_reflns_number_gt                2260
_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 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_cell_refinement       
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_data_reduction        
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury (Macrae at al., 2020)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

# REFINEMENT DATA 

_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)+(0.0353P)²+2.3992P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00084(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2603
_refine_ls_number_parameters     149
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0278
_refine_ls_wR_factor_ref         0.0730
_refine_ls_wR_factor_gt          0.0697
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.339
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.20898(4) 0.56233(4) 0.26073(2) 0.07325(16) Uani 1 1 d . . . . .
C1 C 0.3180(5) 0.4983(6) 0.2115(3) 0.124(2) Uani 1 1 d . . . . .
H11 H 0.3687 0.5576 0.2012 0.186 Uiso 1 1 calc R U . . .
H12 H 0.2748 0.4646 0.1698 0.186 Uiso 1 1 calc R U . . .
H13 H 0.3651 0.4406 0.2390 0.186 Uiso 1 1 calc R U . . .
C2 C 0.3182(5) 0.6656(5) 0.3187(2) 0.1101(19) Uani 1 1 d . . . . .
H21 H 0.2754 0.7141 0.3434 0.165 Uiso 1 1 calc R U . . .
H22 H 0.3575 0.7119 0.2910 0.165 Uiso 1 1 calc R U . . .
H23 H 0.3758 0.6219 0.3504 0.165 Uiso 1 1 calc R U . . .
C3 C 0.1312(4) 0.6721(4) 0.1922(2) 0.0971(15) Uani 1 1 d . . . . .
H31 H 0.1898 0.7144 0.1754 0.146 Uiso 1 1 calc R U . . .
H32 H 0.0844 0.7240 0.2124 0.146 Uiso 1 1 calc R U . . .
H33 H 0.0809 0.6320 0.1551 0.146 Uiso 1 1 calc R U . . .
I1 I 0.09373(2) 0.39585(2) 0.36651(2) 0.06683(13) Uani 1 1 d . . . . .
C4 C 0.0398(3) 0.3043(3) 0.44411(17) 0.0613(9) Uani 1 1 d . . . . .
F1 F 0.1826(2) 0.1612(2) 0.44315(14) 0.0928(7) Uani 1 1 d . . . . .
C5 C 0.0941(4) 0.2029(4) 0.46866(19) 0.0704(10) Uani 1 1 d . . . . .
F2 F 0.1127(3) 0.0445(3) 0.54189(16) 0.1201(10) Uani 1 1 d . U . . .
C6 C 0.0593(5) 0.1435(4) 0.5195(2) 0.0927(16) Uani 1 1 d . . . . .
F3 F -0.0658(4) 0.1261(3) 0.59641(17) 0.1469(14) Uani 1 1 d . U . . .
C7 C -0.0310(6) 0.1855(6) 0.5465(2) 0.1025(18) Uani 1 1 d . U . . .
F4 F -0.1750(3) 0.3248(3) 0.54927(17) 0.1365(13) Uani 1 1 d . U . . .
C8 C -0.0858(5) 0.2849(5) 0.5232(2) 0.0957(16) Uani 1 1 d . . . . .
F5 F -0.1062(3) 0.4418(2) 0.45037(15) 0.0978(8) Uani 1 1 d . . . . .
C9 C -0.0509(4) 0.3442(4) 0.4721(2) 0.0733(11) Uani 1 1 d . . . . .


# MOLECULAR GEOMETRY

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As1 C1 1.920(5) . ?
As1 C2 1.938(5) . ?
As1 C3 1.949(5) . ?
C1 H11 0.9600 . ?
C1 H12 0.9600 . ?
C1 H13 0.9600 . ?
C2 H21 0.9600 . ?
C2 H22 0.9600 . ?
C2 H23 0.9600 . ?
C3 H31 0.9600 . ?
C3 H32 0.9600 . ?
C3 H33 0.9600 . ?
I1 C4 2.096(4) . ?
C4 C9 1.378(5) . ?
C4 C5 1.380(6) . ?
F1 C5 1.335(5) . ?
C5 C6 1.367(6) . ?
F2 C6 1.341(6) . ?
C6 C7 1.372(8) . ?
F3 C7 1.352(6) . ?
C7 C8 1.355(8) . ?
F4 C8 1.342(6) . ?
C8 C9 1.372(6) . ?
F5 C9 1.333(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 As1 C2 97.7(3) . . ?
C1 As1 C3 98.5(2) . . ?
C2 As1 C3 98.8(2) . . ?
As1 C1 H11 109.5 . . ?
As1 C1 H12 109.5 . . ?
H11 C1 H12 109.5 . . ?
As1 C1 H13 109.5 . . ?
H11 C1 H13 109.5 . . ?
H12 C1 H13 109.5 . . ?
As1 C2 H21 109.5 . . ?
As1 C2 H22 109.5 . . ?
H21 C2 H22 109.5 . . ?
As1 C2 H23 109.5 . . ?
H21 C2 H23 109.5 . . ?
H22 C2 H23 109.5 . . ?
As1 C3 H31 109.5 . . ?
As1 C3 H32 109.5 . . ?
H31 C3 H32 109.5 . . ?
As1 C3 H33 109.5 . . ?
H31 C3 H33 109.5 . . ?
H32 C3 H33 109.5 . . ?
C9 C4 C5 118.2(4) . . ?
C9 C4 I1 120.8(3) . . ?
C5 C4 I1 121.0(3) . . ?
F1 C5 C6 118.7(5) . . ?
F1 C5 C4 120.3(4) . . ?
C6 C5 C4 121.0(5) . . ?
F2 C6 C5 119.8(6) . . ?
F2 C6 C7 120.8(5) . . ?
C5 C6 C7 119.5(5) . . ?
F3 C7 C8 120.1(7) . . ?
F3 C7 C6 119.3(6) . . ?
C8 C7 C6 120.6(5) . . ?
F4 C8 C7 120.3(5) . . ?
F4 C8 C9 119.8(6) . . ?
C7 C8 C9 119.8(5) . . ?
F5 C9 C8 118.4(5) . . ?
F5 C9 C4 120.7(4) . . ?
C8 C9 C4 120.9(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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 C4 C5 F1 -179.8(3) . . . . ?
I1 C4 C5 F1 0.0(5) . . . . ?
C9 C4 C5 C6 -0.2(5) . . . . ?
I1 C4 C5 C6 179.6(3) . . . . ?
F1 C5 C6 F2 -1.2(6) . . . . ?
C4 C5 C6 F2 179.2(3) . . . . ?
F1 C5 C6 C7 179.7(4) . . . . ?
C4 C5 C6 C7 0.0(6) . . . . ?
F2 C6 C7 F3 0.2(7) . . . . ?
C5 C6 C7 F3 179.4(4) . . . . ?
F2 C6 C7 C8 -179.1(4) . . . . ?
C5 C6 C7 C8 0.1(7) . . . . ?
F3 C7 C8 F4 -0.1(7) . . . . ?
C6 C7 C8 F4 179.3(4) . . . . ?
F3 C7 C8 C9 -179.3(4) . . . . ?
C6 C7 C8 C9 0.0(7) . . . . ?
F4 C8 C9 F5 1.0(6) . . . . ?
C7 C8 C9 F5 -179.8(4) . . . . ?
F4 C8 C9 C4 -179.4(4) . . . . ?
C7 C8 C9 C4 -0.2(6) . . . . ?
C5 C4 C9 F5 179.9(3) . . . . ?
I1 C4 C9 F5 0.0(5) . . . . ?
C5 C4 C9 C8 0.3(5) . . . . ?
I1 C4 C9 C8 -179.6(3) . . . . ?

_refine_diff_density_max         0.560
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.067


####################################################################### 
# 
# 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_Me3As_C6F5I_150K
_database_code_depnum_ccdc_archive 'CCDC 2057071'
_audit_update_record             
;
2021-01-18 deposited with the CCDC.	2021-12-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H9 As, C6 F5 I'
_chemical_formula_sum            'C9 H9 As F5 I'
_chemical_formula_weight         413.98

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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_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                   11.4664(3)
_cell_length_b                   11.5939(2)
_cell_length_c                   20.0447(4)
_cell_angle_alpha                90
_cell_angle_beta                 102.752(2)
_cell_angle_gamma                90
_cell_volume                     2599.02(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    150.0(1)
_cell_measurement_reflns_used    10174
_cell_measurement_theta_min      2.08
_cell_measurement_theta_max      29.84

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.116
_exptl_crystal_F_000             1552
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    5.022
_shelx_estimated_absorpt_T_min   0.31
_shelx_estimated_absorpt_T_max   0.43
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.01
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?

# EXPERIMENTAL DATA

_exptl_special_details           
; 
Data were collected for the in-situ low-temperature cocrystallized
single crystal. 
;
_diffrn_ambient_temperature      150.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 8.0951
_diffrn_reflns_number            18082
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.083
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2551
_reflns_number_gt                2384
_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 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_cell_refinement       
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_data_reduction        
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury (Macrae at al., 2020)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

# REFINEMENT DATA 

_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)+(0.0228P)²+2.6966P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00028(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2551
_refine_ls_number_parameters     149
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0202
_refine_ls_wR_factor_ref         0.0498
_refine_ls_wR_factor_gt          0.0488
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.446
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.20695(3) 0.56440(3) 0.25991(2) 0.04973(10) Uani 1 1 d . . . . .
C1 C 0.3188(4) 0.4984(4) 0.2110(2) 0.0834(11) Uani 1 1 d . . . . .
H11 H 0.3617 0.5591 0.1944 0.125 Uiso 1 1 calc R U . . .
H12 H 0.2760 0.4536 0.1732 0.125 Uiso 1 1 calc R U . . .
H13 H 0.3743 0.4497 0.2413 0.125 Uiso 1 1 calc R U . . .
C2 C 0.3165(4) 0.6683(3) 0.31864(16) 0.0751(11) Uani 1 1 d . . . . .
H21 H 0.2724 0.7182 0.3423 0.113 Uiso 1 1 calc R U . . .
H22 H 0.3583 0.7138 0.2914 0.113 Uiso 1 1 calc R U . . .
H23 H 0.3730 0.6243 0.3513 0.113 Uiso 1 1 calc R U . . .
C3 C 0.1302(3) 0.6751(3) 0.19089(17) 0.0649(9) Uani 1 1 d . . . . .
H31 H 0.1903 0.7196 0.1760 0.097 Uiso 1 1 calc R U . . .
H32 H 0.0799 0.7255 0.2101 0.097 Uiso 1 1 calc R U . . .
H33 H 0.0827 0.6346 0.1526 0.097 Uiso 1 1 calc R U . . .
I1 I 0.09308(2) 0.39854(2) 0.36546(2) 0.04391(8) Uani 1 1 d . . . . .
C4 C 0.0402(2) 0.3051(2) 0.44357(13) 0.0416(6) Uani 1 1 d . . . . .
F1 F 0.18473(16) 0.16143(16) 0.44156(10) 0.0652(5) Uani 1 1 d . . . . .
C5 C 0.0953(3) 0.2033(3) 0.46759(14) 0.0499(7) Uani 1 1 d . . . . .
F2 F 0.1152(2) 0.04204(19) 0.54080(12) 0.0960(8) Uani 1 1 d . U . . .
C6 C 0.0613(3) 0.1419(3) 0.51903(17) 0.0673(10) Uani 1 1 d . . . . .
F3 F -0.0643(3) 0.1226(2) 0.59599(12) 0.1069(8) Uani 1 1 d . U . . .
C7 C -0.0305(4) 0.1838(4) 0.54633(16) 0.0786(13) Uani 1 1 d . . . . .
F4 F -0.1763(2) 0.3236(2) 0.55020(12) 0.1029(9) Uani 1 1 d . U . . .
C8 C -0.0866(3) 0.2845(4) 0.52347(17) 0.0701(10) Uani 1 1 d . . . . .
F5 F -0.10821(17) 0.44281(17) 0.45096(10) 0.0680(5) Uani 1 1 d . . . . .
C9 C -0.0510(3) 0.3449(3) 0.47233(15) 0.0530(7) Uani 1 1 d . . . . .


# MOLECULAR GEOMETRY

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As1 C1 1.936(4) . ?
As1 C2 1.939(3) . ?
As1 C3 1.949(3) . ?
C1 H11 0.9600 . ?
C1 H12 0.9600 . ?
C1 H13 0.9600 . ?
C2 H21 0.9600 . ?
C2 H22 0.9600 . ?
C2 H23 0.9600 . ?
C3 H31 0.9600 . ?
C3 H32 0.9600 . ?
C3 H33 0.9600 . ?
I1 C4 2.100(3) . ?
C4 C5 1.375(4) . ?
C4 C9 1.380(4) . ?
F1 C5 1.340(4) . ?
C5 C6 1.379(4) . ?
F2 C6 1.339(4) . ?
C6 C7 1.378(6) . ?
F3 C7 1.347(4) . ?
C7 C8 1.363(6) . ?
F4 C8 1.339(4) . ?
C8 C9 1.375(5) . ?
F5 C9 1.334(4) . ?

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
C1 As1 C2 98.05(18) . . ?
C1 As1 C3 98.44(16) . . ?
C2 As1 C3 98.77(16) . . ?
As1 C1 H11 109.5 . . ?
As1 C1 H12 109.5 . . ?
H11 C1 H12 109.5 . . ?
As1 C1 H13 109.5 . . ?
H11 C1 H13 109.5 . . ?
H12 C1 H13 109.5 . . ?
As1 C2 H21 109.5 . . ?
As1 C2 H22 109.5 . . ?
H21 C2 H22 109.5 . . ?
As1 C2 H23 109.5 . . ?
H21 C2 H23 109.5 . . ?
H22 C2 H23 109.5 . . ?
As1 C3 H31 109.5 . . ?
As1 C3 H32 109.5 . . ?
H31 C3 H32 109.5 . . ?
As1 C3 H33 109.5 . . ?
H31 C3 H33 109.5 . . ?
H32 C3 H33 109.5 . . ?
C5 C4 C9 118.2(3) . . ?
C5 C4 I1 121.2(2) . . ?
C9 C4 I1 120.6(2) . . ?
F1 C5 C4 120.5(3) . . ?
F1 C5 C6 118.1(3) . . ?
C4 C5 C6 121.4(3) . . ?
F2 C6 C7 120.9(3) . . ?
F2 C6 C5 120.2(4) . . ?
C7 C6 C5 118.8(3) . . ?
F3 C7 C8 120.6(4) . . ?
F3 C7 C6 118.5(4) . . ?
C8 C7 C6 120.9(3) . . ?
F4 C8 C7 120.2(4) . . ?
F4 C8 C9 120.4(4) . . ?
C7 C8 C9 119.4(4) . . ?
F5 C9 C8 117.8(3) . . ?
F5 C9 C4 121.0(3) . . ?
C8 C9 C4 121.2(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 C4 C5 F1 -179.7(2) . . . . ?
I1 C4 C5 F1 0.1(3) . . . . ?
C9 C4 C5 C6 0.0(4) . . . . ?
I1 C4 C5 C6 179.8(2) . . . . ?
F1 C5 C6 F2 -1.4(4) . . . . ?
C4 C5 C6 F2 179.0(2) . . . . ?
F1 C5 C6 C7 -180.0(3) . . . . ?
C4 C5 C6 C7 0.4(4) . . . . ?
F2 C6 C7 F3 0.6(5) . . . . ?
C5 C6 C7 F3 179.2(3) . . . . ?
F2 C6 C7 C8 -179.0(3) . . . . ?
C5 C6 C7 C8 -0.4(5) . . . . ?
F3 C7 C8 F4 -0.1(5) . . . . ?
C6 C7 C8 F4 179.5(3) . . . . ?
F3 C7 C8 C9 -179.5(3) . . . . ?
C6 C7 C8 C9 0.2(5) . . . . ?
F4 C8 C9 F5 0.3(4) . . . . ?
C7 C8 C9 F5 179.7(3) . . . . ?
F4 C8 C9 C4 -179.1(3) . . . . ?
C7 C8 C9 C4 0.2(5) . . . . ?
C5 C4 C9 F5 -179.7(2) . . . . ?
I1 C4 C9 F5 0.5(4) . . . . ?
C5 C4 C9 C8 -0.3(4) . . . . ?
I1 C4 C9 C8 179.9(2) . . . . ?

_refine_diff_density_max         0.582
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.059


####################################################################### 
# 
# 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_Me3As_100K
_database_code_depnum_ccdc_archive 'CCDC 2057065'
_audit_update_record             
;
2021-01-18 deposited with the CCDC.	2021-12-01 downloaded from the CCDC.
;

# CHEMICAL DATA

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H9 As'
_chemical_formula_sum            'C3 H9 As'
_chemical_formula_weight         120.02

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'

# CRYSTAL DATA

_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_H-M_alt        'C m c 21'
_space_group_name_Hall           'C 2c -2'

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

_cell_length_a                   9.2883(2)
_cell_length_b                   10.9515(3)
_cell_length_c                   5.18635(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     527.56(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.0(1)
_cell_measurement_reflns_used    12716
_cell_measurement_theta_min      2.87
_cell_measurement_theta_max      35.62

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_F_000             240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    6.263
_shelx_estimated_absorpt_T_min   0.37
_shelx_estimated_absorpt_T_max   0.57
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.02
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?


# EXPERIMENTAL DATA

_exptl_special_details           
; 
Data were collected for the in-situ low-temperature crystallized
single crystal. 
;
_diffrn_ambient_temperature      100.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 8.0951
_diffrn_reflns_number            12544
_diffrn_reflns_av_unetI/netI     0.0113
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         2.876
_diffrn_reflns_theta_max         25.967
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             551
_reflns_number_gt                549
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.786
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_cell_refinement       
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_data_reduction        
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury (Macrae at al., 2020)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

# REFINEMENT DATA 

_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0387P)²+0.1850P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.17(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         551
_refine_ls_number_parameters     29
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0192
_refine_ls_R_factor_gt           0.0191
_refine_ls_wR_factor_ref         0.0498
_refine_ls_wR_factor_gt          0.0497
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.5000 0.29570(3) 0.35345(2) 0.02083(19) Uani 1 2 d DS T P . .
C1 C 0.3426(4) 0.3669(3) 0.1507(7) 0.0273(8) Uani 1 1 d . . . . .
H11 H 0.3589 0.3517 -0.0292 0.041 Uiso 1 1 calc R U . . .
H12 H 0.3388 0.4534 0.1804 0.041 Uiso 1 1 calc R U . . .
H13 H 0.2529 0.3306 0.2018 0.041 Uiso 1 1 calc R U . . .
C2 C 0.5000 0.1350(3) 0.1858(5) 0.0298(11) Uani 1 2 d DS T P . .
H21 H 0.5000 0.1454(2) 0.0020(4) 0.045 Uiso 1 2 d DS U P . .
H22 H 0.58441(2) 0.09048(8) 0.2368(6) 0.045 Uiso 1 1 d D U . . .


# MOLECULAR GEOMETRY

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As1 C1 1.963(4) 3_655 ?
As1 C1 1.963(4) . ?
As1 C2 1.963(3) . ?
C1 H11 0.9600 . ?
C1 H12 0.9600 . ?
C1 H13 0.9600 . ?
C2 H21 0.9601(14) . ?
C2 H22 0.9601(12) . ?

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
C1 As1 C1 96.3(2) 3_655 . ?
C1 As1 C2 96.85(12) 3_655 . ?
C1 As1 C2 96.85(12) . . ?
As1 C1 H11 109.5 . . ?
As1 C1 H12 109.5 . . ?
H11 C1 H12 109.5 . . ?
As1 C1 H13 109.5 . . ?
H11 C1 H13 109.5 . . ?
H12 C1 H13 109.5 . . ?
As1 C2 H21 109.46(18) . . ?
As1 C2 H22 109.46(15) . . ?
H21 C2 H22 109.49(15) . . ?

_refine_diff_density_max         0.287
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.051


####################################################################### 
# 
# 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_Me3Sb_100K
_database_code_depnum_ccdc_archive 'CCDC 2057068'
_audit_update_record             
;
2021-01-18 deposited with the CCDC.	2021-12-01 downloaded from the CCDC.
;

# CHEMICAL DATA

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H9 Sb'
_chemical_formula_sum            'C3 H9 Sb'
_chemical_formula_weight         166.86

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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   6.04482(9)
_cell_length_b                   11.14435(16)
_cell_length_c                   8.48341(13)
_cell_angle_alpha                90
_cell_angle_beta                 96.8289(14)
_cell_angle_gamma                90
_cell_volume                     567.436(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.0(1)
_cell_measurement_reflns_used    7434
_cell_measurement_theta_min      1.83
_cell_measurement_theta_max      32.04

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.953
_exptl_crystal_F_000             312
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_exptl_absorpt_coefficient_mu    4.695
_shelx_estimated_absorpt_T_min   0.33
_shelx_estimated_absorpt_T_max   0.33
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.46
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?


# EXPERIMENTAL DATA

_exptl_special_details           
; 
Data were collected for the in-situ low-temperature crystallized
single crystal. 
;
_diffrn_ambient_temperature      100.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 8.0951
_diffrn_reflns_number            7411
_diffrn_reflns_av_unetI/netI     0.0130
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         4.333
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.984
_reflns_number_total             1103
_reflns_number_gt                1089
_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 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_cell_refinement       
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_data_reduction        
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury (Macrae at al., 2020)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

# REFINEMENT DATA 

_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)+(0.0103P)²+0.1446P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0144(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1103
_refine_ls_number_parameters     41
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0126
_refine_ls_R_factor_gt           0.0123
_refine_ls_wR_factor_ref         0.0271
_refine_ls_wR_factor_gt          0.0270
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_restrained_S_all      1.171
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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 0.47746(2) 0.33880(2) 0.42027(2) 0.02075(7) Uani 1 1 d . . . . .
C1 C 0.5134(3) 0.41639(18) 0.1931(2) 0.0270(4) Uani 1 1 d . . . . .
H11 H 0.4806 0.5006 0.1953 0.040 Uiso 1 1 calc R U . . .
H12 H 0.4122 0.3780 0.1128 0.040 Uiso 1 1 calc R U . . .
H13 H 0.6635 0.4052 0.1696 0.040 Uiso 1 1 calc R U . . .
C2 C 0.1194(4) 0.34451(18) 0.3851(3) 0.0313(5) Uani 1 1 d . . . . .
H21 H 0.0668 0.3107 0.2834 0.047 Uiso 1 1 calc R U . . .
H22 H 0.0703 0.4263 0.3891 0.047 Uiso 1 1 calc R U . . .
H23 H 0.0612 0.2991 0.4671 0.047 Uiso 1 1 calc R U . . .
C3 C 0.4998(4) 0.15587(16) 0.3418(3) 0.0301(5) Uani 1 1 d . . . . .
H31 H 0.6492 0.1396 0.3202 0.045 Uiso 1 1 calc R U . . .
H32 H 0.3987 0.1439 0.2470 0.045 Uiso 1 1 calc R U . . .
H33 H 0.4616 0.1026 0.4233 0.045 Uiso 1 1 calc R U . . .


# MOLECULAR GEOMETRY

_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 C1 2.1468(19) . ?
Sb1 C2 2.151(2) . ?
Sb1 C3 2.1538(18) . ?
C1 H11 0.9600 . ?
C1 H12 0.9600 . ?
C1 H13 0.9600 . ?
C2 H21 0.9600 . ?
C2 H22 0.9600 . ?
C2 H23 0.9600 . ?
C3 H31 0.9600 . ?
C3 H32 0.9600 . ?
C3 H33 0.9600 . ?

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
C1 Sb1 C2 94.09(8) . . ?
C1 Sb1 C3 94.99(8) . . ?
C2 Sb1 C3 94.84(8) . . ?
Sb1 C1 H11 109.5 . . ?
Sb1 C1 H12 109.5 . . ?
H11 C1 H12 109.5 . . ?
Sb1 C1 H13 109.5 . . ?
H11 C1 H13 109.5 . . ?
H12 C1 H13 109.5 . . ?
Sb1 C2 H21 109.5 . . ?
Sb1 C2 H22 109.5 . . ?
H21 C2 H22 109.5 . . ?
Sb1 C2 H23 109.5 . . ?
H21 C2 H23 109.5 . . ?
H22 C2 H23 109.5 . . ?
Sb1 C3 H31 109.5 . . ?
Sb1 C3 H32 109.5 . . ?
H31 C3 H32 109.5 . . ?
Sb1 C3 H33 109.5 . . ?
H31 C3 H33 109.5 . . ?
H32 C3 H33 109.5 . . ?

_refine_diff_density_max         0.408
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.055



#############################################################################


####################################################################### 
# 
# 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_Me3Sb_C6F5I_180K
_database_code_depnum_ccdc_archive 'CCDC 2057074'
_audit_update_record             
;
2021-01-18 deposited with the CCDC.	2021-12-01 downloaded from the CCDC.
;

# CHEMICAL DATA

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H9 Sb, C6 F5 I'
_chemical_formula_sum            'C9 H9 F5 I Sb'
_chemical_formula_weight         460.82

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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

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

_cell_length_a                   20.1543(14)
_cell_length_b                   6.0578(3)
_cell_length_c                   23.5026(14)
_cell_angle_alpha                90
_cell_angle_beta                 108.230(7)
_cell_angle_gamma                90
_cell_volume                     2725.4(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    180.0(1)
_cell_measurement_reflns_used    8339
_cell_measurement_theta_min      2.05
_cell_measurement_theta_max      30.33

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.246
_exptl_crystal_F_000             1696
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    4.320
_shelx_estimated_absorpt_T_min   0.67
_shelx_estimated_absorpt_T_max   0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.25
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?


# EXPERIMENTAL DATA

_exptl_special_details           
; 
Data were collected for the in-situ low-temperature cocrystallized
single crystal. 
;
_diffrn_ambient_temperature      180.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 8.0951
_diffrn_reflns_number            18159
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.128
_diffrn_reflns_theta_max         25.996
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2686
_reflns_number_gt                2423
_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 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_cell_refinement       
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_data_reduction        
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury (Macrae at al., 2020)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

# REFINEMENT DATA 

_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)+(0.0265P)²+2.5261P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2686
_refine_ls_number_parameters     148
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0270
_refine_ls_wR_factor_ref         0.0624
_refine_ls_wR_factor_gt          0.0599
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      1.096
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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 0.27263(2) 0.40677(5) 0.39554(2) 0.05071(10) Uani 1 1 d . . . . .
C1 C 0.1841(3) 0.1990(10) 0.3814(4) 0.112(2) Uani 1 1 d . U . . .
H11 H 0.1719 0.1365 0.3420 0.169 Uiso 1 1 calc R U . . .
H12 H 0.1455 0.2840 0.3853 0.169 Uiso 1 1 calc R U . . .
H13 H 0.1948 0.0827 0.4106 0.169 Uiso 1 1 calc R U . . .
C2 C 0.3321(3) 0.1792(8) 0.3622(2) 0.0681(13) Uani 1 1 d . . . . .
H21 H 0.3711 0.2544 0.3558 0.102 Uiso 1 1 calc R U . . .
H22 H 0.3032 0.1183 0.3249 0.102 Uiso 1 1 calc R U . . .
H23 H 0.3488 0.0625 0.3907 0.102 Uiso 1 1 calc R U . . .
C3 C 0.2308(4) 0.5832(9) 0.3149(3) 0.101(2) Uani 1 1 d . . . . .
H31 H 0.2047 0.4844 0.2840 0.152 Uiso 1 1 calc R U . . .
H32 H 0.2681 0.6478 0.3033 0.152 Uiso 1 1 calc R U . . .
H33 H 0.2005 0.6977 0.3206 0.152 Uiso 1 1 calc R U . . .
I1 I 0.37495(2) 0.73529(4) 0.51486(2) 0.04552(10) Uani 1 1 d . . . . .
C4 C 0.4465(2) 0.9269(5) 0.58016(15) 0.0379(8) Uani 1 1 d . . . . .
F1 F 0.44724(14) 0.6694(4) 0.65566(10) 0.0589(6) Uani 1 1 d . . . . .
C5 C 0.4700(2) 0.8608(6) 0.63938(16) 0.0415(8) Uani 1 1 d . . . . .
F2 F 0.53891(16) 0.9129(4) 0.73938(10) 0.0724(8) Uani 1 1 d . . . . .
C6 C 0.5158(2) 0.9851(7) 0.68260(16) 0.0494(9) Uani 1 1 d . . . . .
F3 F 0.58450(14) 1.3054(4) 0.70869(11) 0.0685(7) Uani 1 1 d . . . . .
C7 C 0.5392(2) 1.1821(7) 0.66715(18) 0.0479(9) Uani 1 1 d . . . . .
F4 F 0.54081(13) 1.4439(3) 0.59399(12) 0.0614(6) Uani 1 1 d . . . . .
C8 C 0.5172(2) 1.2521(6) 0.60842(19) 0.0454(9) Uani 1 1 d . . . . .
F5 F 0.45127(13) 1.1949(3) 0.50903(9) 0.0529(6) Uani 1 1 d . . . . .
C9 C 0.4715(2) 1.1237(6) 0.56580(16) 0.0393(8) Uani 1 1 d . . . . .


# MOLECULAR GEOMETRY

_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 C3 2.109(5) . ?
Sb1 C1 2.124(6) . ?
Sb1 C2 2.131(5) . ?
C1 H11 0.9600 . ?
C1 H12 0.9600 . ?
C1 H13 0.9600 . ?
C2 H21 0.9600 . ?
C2 H22 0.9600 . ?
C2 H23 0.9600 . ?
C3 H31 0.9600 . ?
C3 H32 0.9600 . ?
C3 H33 0.9600 . ?
I1 C4 2.097(3) . ?
C4 C9 1.377(5) . ?
C4 C5 1.382(5) . ?
F1 C5 1.346(4) . ?
C5 C6 1.365(5) . ?
F2 C6 1.342(4) . ?
C6 C7 1.373(6) . ?
F3 C7 1.337(4) . ?
C7 C8 1.378(6) . ?
F4 C8 1.338(4) . ?
C8 C9 1.371(5) . ?
F5 C9 1.339(4) . ?

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
C3 Sb1 C1 94.6(3) . . ?
C3 Sb1 C2 96.3(2) . . ?
C1 Sb1 C2 95.8(2) . . ?
Sb1 C1 H11 109.5 . . ?
Sb1 C1 H12 109.5 . . ?
H11 C1 H12 109.5 . . ?
Sb1 C1 H13 109.5 . . ?
H11 C1 H13 109.5 . . ?
H12 C1 H13 109.5 . . ?
Sb1 C2 H21 109.5 . . ?
Sb1 C2 H22 109.5 . . ?
H21 C2 H22 109.5 . . ?
Sb1 C2 H23 109.5 . . ?
H21 C2 H23 109.5 . . ?
H22 C2 H23 109.5 . . ?
Sb1 C3 H31 109.5 . . ?
Sb1 C3 H32 109.5 . . ?
H31 C3 H32 109.5 . . ?
Sb1 C3 H33 109.5 . . ?
H31 C3 H33 109.5 . . ?
H32 C3 H33 109.5 . . ?
C9 C4 C5 117.5(3) . . ?
C9 C4 I1 121.4(3) . . ?
C5 C4 I1 121.1(3) . . ?
F1 C5 C6 118.3(3) . . ?
F1 C5 C4 119.8(3) . . ?
C6 C5 C4 121.9(4) . . ?
F2 C6 C5 120.3(4) . . ?
F2 C6 C7 120.3(4) . . ?
C5 C6 C7 119.4(3) . . ?
F3 C7 C6 120.3(4) . . ?
F3 C7 C8 119.4(4) . . ?
C6 C7 C8 120.2(3) . . ?
F4 C8 C9 121.2(4) . . ?
F4 C8 C7 119.5(4) . . ?
C9 C8 C7 119.3(3) . . ?
F5 C9 C8 118.1(3) . . ?
F5 C9 C4 120.2(3) . . ?
C8 C9 C4 121.7(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 C4 C5 F1 -179.8(3) . . . . ?
I1 C4 C5 F1 0.7(5) . . . . ?
C9 C4 C5 C6 0.5(6) . . . . ?
I1 C4 C5 C6 -179.1(3) . . . . ?
F1 C5 C6 F2 2.1(6) . . . . ?
C4 C5 C6 F2 -178.2(4) . . . . ?
F1 C5 C6 C7 -179.4(3) . . . . ?
C4 C5 C6 C7 0.4(6) . . . . ?
F2 C6 C7 F3 -0.9(6) . . . . ?
C5 C6 C7 F3 -179.4(4) . . . . ?
F2 C6 C7 C8 177.7(4) . . . . ?
C5 C6 C7 C8 -0.8(6) . . . . ?
F3 C7 C8 F4 -1.0(6) . . . . ?
C6 C7 C8 F4 -179.6(3) . . . . ?
F3 C7 C8 C9 179.1(3) . . . . ?
C6 C7 C8 C9 0.5(6) . . . . ?
F4 C8 C9 F5 0.4(5) . . . . ?
C7 C8 C9 F5 -179.7(3) . . . . ?
F4 C8 C9 C4 -179.6(3) . . . . ?
C7 C8 C9 C4 0.3(6) . . . . ?
C5 C4 C9 F5 179.2(3) . . . . ?
I1 C4 C9 F5 -1.3(5) . . . . ?
C5 C4 C9 C8 -0.8(5) . . . . ?
I1 C4 C9 C8 178.7(3) . . . . ?

_refine_diff_density_max         0.890
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.090


####################################################################### 
# 
# 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_Me3As_C6F5I_100K
_database_code_depnum_ccdc_archive 'CCDC 2057072'
_audit_update_record             
;
2021-01-18 deposited with the CCDC.	2021-12-01 downloaded from the CCDC.
;

# CHEMICAL DATA

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H9 As, C6 F5 I'
_chemical_formula_sum            'C9 H9 As F5 I'
_chemical_formula_weight         413.98

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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_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                   11.3040(2)
_cell_length_b                   11.5876(2)
_cell_length_c                   20.0586(4)
_cell_angle_alpha                90
_cell_angle_beta                 102.512(2)
_cell_angle_gamma                90
_cell_volume                     2565.00(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    100.0(1)
_cell_measurement_reflns_used    12065
_cell_measurement_theta_min      2.07
_cell_measurement_theta_max      31.69

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.144
_exptl_crystal_F_000             1552
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    5.089
_shelx_estimated_absorpt_T_min   0.310
_shelx_estimated_absorpt_T_max   0.429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.03
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?


# EXPERIMENTAL DATA

_exptl_special_details           
; 
Data were collected for the in-situ low-temperature cocrystallized
single crystal. 
;
_diffrn_ambient_temperature      100.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 8.0951
_diffrn_reflns_number            17720
_diffrn_reflns_av_unetI/netI     0.0147
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.080
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2510
_reflns_number_gt                2386
_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 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_cell_refinement       
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_data_reduction        
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury (Macrae at al., 2020)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

# REFINEMENT DATA 

_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)+(0.0152P)²+4.0282P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2510
_refine_ls_number_parameters     148
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0200
_refine_ls_R_factor_gt           0.0183
_refine_ls_wR_factor_ref         0.0425
_refine_ls_wR_factor_gt          0.0419
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_restrained_S_all      1.366
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.20477(3) 0.56571(2) 0.25922(2) 0.03776(8) Uani 1 1 d . . . . .
C1 C 0.3175(3) 0.4962(3) 0.21042(17) 0.0608(9) Uani 1 1 d . . . . .
H11 H 0.3608 0.5559 0.1925 0.091 Uiso 1 1 calc R U . . .
H12 H 0.2736 0.4500 0.1735 0.091 Uiso 1 1 calc R U . . .
H13 H 0.3740 0.4485 0.2411 0.091 Uiso 1 1 calc R U . . .
C2 C 0.3184(3) 0.6680(3) 0.31772(15) 0.0544(8) Uani 1 1 d . . . . .
H21 H 0.2748 0.7199 0.3409 0.082 Uiso 1 1 calc R U . . .
H22 H 0.3627 0.7114 0.2904 0.082 Uiso 1 1 calc R U . . .
H23 H 0.3739 0.6231 0.3507 0.082 Uiso 1 1 calc R U . . .
C3 C 0.1295(3) 0.6773(3) 0.19015(15) 0.0470(7) Uani 1 1 d . . . . .
H31 H 0.1910 0.7253 0.1782 0.070 Uiso 1 1 calc R U . . .
H32 H 0.0736 0.7243 0.2079 0.070 Uiso 1 1 calc R U . . .
H33 H 0.0869 0.6371 0.1503 0.070 Uiso 1 1 calc R U . . .
I1 I 0.09173(2) 0.40086(2) 0.36459(2) 0.03204(6) Uani 1 1 d . . . . .
C4 C 0.0404(2) 0.3056(2) 0.44284(12) 0.0329(6) Uani 1 1 d . . . . .
F1 F 0.18701(15) 0.16216(14) 0.43824(10) 0.0520(4) Uani 1 1 d . . . . .
C5 C 0.0974(3) 0.2033(2) 0.46550(14) 0.0406(7) Uani 1 1 d . . . . .
F2 F 0.1194(2) 0.04005(17) 0.53769(10) 0.0803(8) Uani 1 1 d . . . . .
C6 C 0.0643(3) 0.1404(3) 0.51713(16) 0.0572(10) Uani 1 1 d . . . . .
F3 F -0.0609(3) 0.1189(2) 0.59576(10) 0.0946(8) Uani 1 1 d . U . . .
C7 C -0.0279(4) 0.1809(4) 0.54606(15) 0.0665(12) Uani 1 1 d . . . . .
F4 F -0.1758(2) 0.3198(2) 0.55244(11) 0.0901(8) Uani 1 1 d . . . . .
C8 C -0.0856(3) 0.2819(3) 0.52435(16) 0.0592(10) Uani 1 1 d . . . . .
F5 F -0.11004(16) 0.44219(16) 0.45287(9) 0.0536(4) Uani 1 1 d . . . . .
C9 C -0.0508(3) 0.3438(3) 0.47311(14) 0.0425(7) Uani 1 1 d . . . . .


# MOLECULAR GEOMETRY

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As1 C1 1.942(3) . ?
As1 C2 1.944(3) . ?
As1 C3 1.950(3) . ?
C1 H11 0.9600 . ?
C1 H12 0.9600 . ?
C1 H13 0.9600 . ?
C2 H21 0.9600 . ?
C2 H22 0.9600 . ?
C2 H23 0.9600 . ?
C3 H31 0.9600 . ?
C3 H32 0.9600 . ?
C3 H33 0.9600 . ?
I1 C4 2.101(2) . ?
C4 C9 1.378(4) . ?
C4 C5 1.379(4) . ?
F1 C5 1.339(3) . ?
C5 C6 1.382(4) . ?
F2 C6 1.342(4) . ?
C6 C7 1.380(6) . ?
F3 C7 1.346(4) . ?
C7 C8 1.364(6) . ?
F4 C8 1.342(4) . ?
C8 C9 1.379(4) . ?
F5 C9 1.339(4) . ?

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
C1 As1 C2 97.87(15) . . ?
C1 As1 C3 98.61(14) . . ?
C2 As1 C3 98.88(14) . . ?
As1 C1 H11 109.5 . . ?
As1 C1 H12 109.5 . . ?
H11 C1 H12 109.5 . . ?
As1 C1 H13 109.5 . . ?
H11 C1 H13 109.5 . . ?
H12 C1 H13 109.5 . . ?
As1 C2 H21 109.5 . . ?
As1 C2 H22 109.5 . . ?
H21 C2 H22 109.5 . . ?
As1 C2 H23 109.5 . . ?
H21 C2 H23 109.5 . . ?
H22 C2 H23 109.5 . . ?
As1 C3 H31 109.5 . . ?
As1 C3 H32 109.5 . . ?
H31 C3 H32 109.5 . . ?
As1 C3 H33 109.5 . . ?
H31 C3 H33 109.5 . . ?
H32 C3 H33 109.5 . . ?
C9 C4 C5 118.1(3) . . ?
C9 C4 I1 121.0(2) . . ?
C5 C4 I1 120.9(2) . . ?
F1 C5 C4 120.8(2) . . ?
F1 C5 C6 118.0(3) . . ?
C4 C5 C6 121.2(3) . . ?
F2 C6 C7 120.5(3) . . ?
F2 C6 C5 120.3(4) . . ?
C7 C6 C5 119.2(3) . . ?
F3 C7 C8 120.2(4) . . ?
F3 C7 C6 119.1(4) . . ?
C8 C7 C6 120.6(3) . . ?
F4 C8 C7 120.1(3) . . ?
F4 C8 C9 120.5(4) . . ?
C7 C8 C9 119.4(3) . . ?
F5 C9 C4 120.8(3) . . ?
F5 C9 C8 117.7(3) . . ?
C4 C9 C8 121.5(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 C4 C5 F1 -179.7(2) . . . . ?
I1 C4 C5 F1 0.1(3) . . . . ?
C9 C4 C5 C6 0.0(4) . . . . ?
I1 C4 C5 C6 179.78(19) . . . . ?
F1 C5 C6 F2 -1.5(4) . . . . ?
C4 C5 C6 F2 178.9(2) . . . . ?
F1 C5 C6 C7 -180.0(2) . . . . ?
C4 C5 C6 C7 0.4(4) . . . . ?
F2 C6 C7 F3 0.7(4) . . . . ?
C5 C6 C7 F3 179.2(2) . . . . ?
F2 C6 C7 C8 -178.8(3) . . . . ?
C5 C6 C7 C8 -0.3(4) . . . . ?
F3 C7 C8 F4 -0.1(4) . . . . ?
C6 C7 C8 F4 179.4(3) . . . . ?
F3 C7 C8 C9 -179.7(3) . . . . ?
C6 C7 C8 C9 -0.2(5) . . . . ?
C5 C4 C9 F5 -179.5(2) . . . . ?
I1 C4 C9 F5 0.7(3) . . . . ?
C5 C4 C9 C8 -0.4(4) . . . . ?
I1 C4 C9 C8 179.8(2) . . . . ?
F4 C8 C9 F5 0.0(4) . . . . ?
C7 C8 C9 F5 179.6(3) . . . . ?
F4 C8 C9 C4 -179.0(3) . . . . ?
C7 C8 C9 C4 0.6(4) . . . . ?

_refine_diff_density_max         0.606
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.061

####################################################################### 
# 
# 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_Me3As_125K
_database_code_depnum_ccdc_archive 'CCDC 2057064'
_audit_update_record             
;
2021-01-18 deposited with the CCDC.	2021-12-01 downloaded from the CCDC.
;

# CHEMICAL DATA

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H9 As'
_chemical_formula_sum            'C3 H9 As'
_chemical_formula_weight         120.02

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'

# CRYSTAL DATA

_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_H-M_alt        'C m c 21'
_space_group_name_Hall           'C 2c -2'

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

_cell_length_a                   9.3043(5)
_cell_length_b                   10.9531(6)
_cell_length_c                   5.1983(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     529.76(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    125.0(1)
_cell_measurement_reflns_used    3427
_cell_measurement_theta_min      3.72
_cell_measurement_theta_max      33.09

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_F_000             240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    6.237
_shelx_estimated_absorpt_T_min   0.37
_shelx_estimated_absorpt_T_max   0.57
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.03
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?


# EXPERIMENTAL DATA

_exptl_special_details           
; 
Data were collected for the in-situ low-temperature crystallized
single crystal. 
;
_diffrn_ambient_temperature      125.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 8.0951
_diffrn_reflns_number            4052
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         2.873
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             554
_reflns_number_gt                550
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.788
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_cell_refinement       
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_data_reduction        
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury (Macrae at al., 2020)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

# REFINEMENT DATA 

_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0984P)²+0.5222P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.16(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         554
_refine_ls_number_parameters     29
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0478
_refine_ls_wR_factor_ref         0.1210
_refine_ls_wR_factor_gt          0.1209
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_restrained_S_all      1.111
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.5000 0.29550(6) 0.35227(2) 0.0269(5) Uani 1 2 d DS T P . .
C1 C 0.3436(9) 0.3671(8) 0.1505(17) 0.0360(18) Uani 1 1 d . . . . .
H11 H 0.3593 0.3509 -0.0288 0.054 Uiso 1 1 calc R U . . .
H12 H 0.3410 0.4537 0.1785 0.054 Uiso 1 1 calc R U . . .
H13 H 0.2538 0.3317 0.2029 0.054 Uiso 1 1 calc R U . . .
C2 C 0.5000 0.1353(3) 0.1853(6) 0.037(3) Uani 1 2 d DS T P . .
H21 H 0.5000 0.1457(2) 0.0020(4) 0.055 Uiso 1 2 d DS U P . .
H22 H 0.58426(2) 0.09077(10) 0.2361(6) 0.055 Uiso 1 1 d D U . . .


# MOLECULAR GEOMETRY

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As1 C2 1.958(3) . ?
As1 C1 1.958(9) . ?
As1 C1 1.958(9) 3_655 ?
C1 H11 0.9600 . ?
C1 H12 0.9600 . ?
C1 H13 0.9600 . ?
C2 H21 0.9601(14) . ?
C2 H22 0.9601(14) . ?

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
C2 As1 C1 97.0(3) . . ?
C2 As1 C1 97.0(3) . 3_655 ?
C1 As1 C1 96.0(5) . 3_655 ?
As1 C1 H11 109.5 . . ?
As1 C1 H12 109.5 . . ?
H11 C1 H12 109.5 . . ?
As1 C1 H13 109.5 . . ?
H11 C1 H13 109.5 . . ?
H12 C1 H13 109.5 . . ?
As1 C2 H21 109.5(2) . . ?
As1 C2 H22 109.46(16) . . ?
H21 C2 H22 109.49(16) . . ?

_refine_diff_density_max         0.326
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.073


####################################################################### 
# 
# 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_Me3Sb_C6F5I_150K
_database_code_depnum_ccdc_archive 'CCDC 2057075'
_audit_update_record             
;
2021-01-18 deposited with the CCDC.	2021-12-01 downloaded from the CCDC.
;

# CHEMICAL DATA

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H9 Sb, C6 F5 I'
_chemical_formula_sum            'C9 H9 F5 I Sb'
_chemical_formula_weight         460.82

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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

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

_cell_length_a                   20.0697(14)
_cell_length_b                   6.0327(3)
_cell_length_c                   23.5298(14)
_cell_angle_alpha                90
_cell_angle_beta                 108.600(7)
_cell_angle_gamma                90
_cell_volume                     2700.1(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    150.0(1)
_cell_measurement_reflns_used    8900
_cell_measurement_theta_min      2.06
_cell_measurement_theta_max      31.70

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.267
_exptl_crystal_F_000             1696
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    4.360
_shelx_estimated_absorpt_T_min   0.67
_shelx_estimated_absorpt_T_max   0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.23
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?


# EXPERIMENTAL DATA

_exptl_special_details           
; 
Data were collected for the in-situ low-temperature cocrystallized
single crystal. 
;
_diffrn_ambient_temperature      150.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 8.0951
_diffrn_reflns_number            17700
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.141
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2656
_reflns_number_gt                2408
_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 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_cell_refinement       
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_data_reduction        
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury (Macrae at al., 2020)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

# REFINEMENT DATA 

_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)+(0.0231P)²+2.6459P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2656
_refine_ls_number_parameters     148
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0252
_refine_ls_wR_factor_ref         0.0565
_refine_ls_wR_factor_gt          0.0543
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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 0.27234(2) 0.40436(4) 0.39539(2) 0.04164(9) Uani 1 1 d . . . . .
C1 C 0.1827(3) 0.1969(9) 0.3808(3) 0.094(2) Uani 1 1 d . . . . .
H11 H 0.1693 0.1380 0.3409 0.142 Uiso 1 1 calc R U . . .
H12 H 0.1445 0.2819 0.3859 0.142 Uiso 1 1 calc R U . . .
H13 H 0.1938 0.0772 0.4092 0.142 Uiso 1 1 calc R U . . .
C2 C 0.3320(2) 0.1744(7) 0.3619(2) 0.0561(11) Uani 1 1 d . . . . .
H21 H 0.3697 0.2511 0.3536 0.084 Uiso 1 1 calc R U . . .
H22 H 0.3021 0.1073 0.3258 0.084 Uiso 1 1 calc R U . . .
H23 H 0.3510 0.0615 0.3914 0.084 Uiso 1 1 calc R U . . .
C3 C 0.2309(3) 0.5834(8) 0.3145(2) 0.0825(17) Uani 1 1 d . . . . .
H31 H 0.2064 0.4837 0.2830 0.124 Uiso 1 1 calc R U . . .
H32 H 0.2685 0.6534 0.3044 0.124 Uiso 1 1 calc R U . . .
H33 H 0.1989 0.6943 0.3194 0.124 Uiso 1 1 calc R U . . .
I1 I 0.37498(2) 0.73317(4) 0.51455(2) 0.03722(9) Uani 1 1 d . . . . .
C4 C 0.44682(19) 0.9265(5) 0.58006(14) 0.0316(7) Uani 1 1 d . . . . .
F1 F 0.44757(13) 0.6693(4) 0.65585(9) 0.0485(6) Uani 1 1 d . . . . .
C5 C 0.4701(2) 0.8618(6) 0.63936(15) 0.0356(8) Uani 1 1 d . . . . .
F2 F 0.53906(14) 0.9163(4) 0.73958(9) 0.0590(7) Uani 1 1 d . . . . .
C6 C 0.5162(2) 0.9871(6) 0.68280(15) 0.0409(9) Uani 1 1 d . . . . .
F3 F 0.58476(13) 1.3101(4) 0.70910(10) 0.0562(6) Uani 1 1 d . . . . .
C7 C 0.5397(2) 1.1852(6) 0.66740(16) 0.0396(9) Uani 1 1 d . . . . .
F4 F 0.54132(12) 1.4464(3) 0.59385(11) 0.0498(6) Uani 1 1 d . . . . .
C8 C 0.5175(2) 1.2539(5) 0.60833(17) 0.0365(8) Uani 1 1 d . . . . .
F5 F 0.45177(12) 1.1946(3) 0.50872(9) 0.0428(5) Uani 1 1 d . . . . .
C9 C 0.47177(19) 1.1240(5) 0.56556(15) 0.0318(7) Uani 1 1 d . . . . .


# MOLECULAR GEOMETRY

_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 C3 2.115(5) . ?
Sb1 C1 2.128(5) . ?
Sb1 C2 2.140(4) . ?
C1 H11 0.9600 . ?
C1 H12 0.9600 . ?
C1 H13 0.9600 . ?
C2 H21 0.9600 . ?
C2 H22 0.9600 . ?
C2 H23 0.9600 . ?
C3 H31 0.9600 . ?
C3 H32 0.9600 . ?
C3 H33 0.9600 . ?
I1 C4 2.097(3) . ?
C4 C9 1.377(5) . ?
C4 C5 1.379(5) . ?
F1 C5 1.348(4) . ?
C5 C6 1.367(5) . ?
F2 C6 1.337(4) . ?
C6 C7 1.375(6) . ?
F3 C7 1.335(4) . ?
C7 C8 1.381(5) . ?
F4 C8 1.341(4) . ?
C8 C9 1.371(5) . ?
F5 C9 1.337(4) . ?

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
C3 Sb1 C1 94.9(3) . . ?
C3 Sb1 C2 96.1(2) . . ?
C1 Sb1 C2 95.9(2) . . ?
Sb1 C1 H11 109.5 . . ?
Sb1 C1 H12 109.5 . . ?
H11 C1 H12 109.5 . . ?
Sb1 C1 H13 109.5 . . ?
H11 C1 H13 109.5 . . ?
H12 C1 H13 109.5 . . ?
Sb1 C2 H21 109.5 . . ?
Sb1 C2 H22 109.5 . . ?
H21 C2 H22 109.5 . . ?
Sb1 C2 H23 109.5 . . ?
H21 C2 H23 109.5 . . ?
H22 C2 H23 109.5 . . ?
Sb1 C3 H31 109.5 . . ?
Sb1 C3 H32 109.5 . . ?
H31 C3 H32 109.5 . . ?
Sb1 C3 H33 109.5 . . ?
H31 C3 H33 109.5 . . ?
H32 C3 H33 109.5 . . ?
C9 C4 C5 117.6(3) . . ?
C9 C4 I1 121.2(2) . . ?
C5 C4 I1 121.2(3) . . ?
F1 C5 C6 118.1(3) . . ?
F1 C5 C4 119.9(3) . . ?
C6 C5 C4 122.0(3) . . ?
F2 C6 C5 120.3(4) . . ?
F2 C6 C7 120.3(3) . . ?
C5 C6 C7 119.4(3) . . ?
F3 C7 C6 120.4(3) . . ?
F3 C7 C8 119.8(3) . . ?
C6 C7 C8 119.8(3) . . ?
F4 C8 C9 121.2(3) . . ?
F4 C8 C7 119.2(3) . . ?
C9 C8 C7 119.6(3) . . ?
F5 C9 C8 118.0(3) . . ?
F5 C9 C4 120.4(3) . . ?
C8 C9 C4 121.6(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 C4 C5 F1 -179.7(3) . . . . ?
I1 C4 C5 F1 1.1(5) . . . . ?
C9 C4 C5 C6 0.1(5) . . . . ?
I1 C4 C5 C6 -179.1(3) . . . . ?
F1 C5 C6 F2 1.5(5) . . . . ?
C4 C5 C6 F2 -178.3(3) . . . . ?
F1 C5 C6 C7 -179.5(3) . . . . ?
C4 C5 C6 C7 0.8(6) . . . . ?
F2 C6 C7 F3 -1.0(6) . . . . ?
C5 C6 C7 F3 -180.0(3) . . . . ?
F2 C6 C7 C8 178.1(3) . . . . ?
C5 C6 C7 C8 -0.9(6) . . . . ?
F3 C7 C8 F4 -0.3(5) . . . . ?
C6 C7 C8 F4 -179.4(3) . . . . ?
F3 C7 C8 C9 179.3(3) . . . . ?
C6 C7 C8 C9 0.3(6) . . . . ?
F4 C8 C9 F5 0.2(5) . . . . ?
C7 C8 C9 F5 -179.4(3) . . . . ?
F4 C8 C9 C4 -179.8(3) . . . . ?
C7 C8 C9 C4 0.6(5) . . . . ?
C5 C4 C9 F5 179.2(3) . . . . ?
I1 C4 C9 F5 -1.6(5) . . . . ?
C5 C4 C9 C8 -0.8(5) . . . . ?
I1 C4 C9 C8 178.4(3) . . . . ?

_refine_diff_density_max         0.651
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.097


####################################################################### 
# 
# 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_Me3Sb_170K
_database_code_depnum_ccdc_archive 'CCDC 2057066'
_audit_update_record             
;
2021-01-18 deposited with the CCDC.	2021-12-01 downloaded from the CCDC.
;

# CHEMICAL DATA

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H9 Sb'
_chemical_formula_sum            'C3 H9 Sb'
_chemical_formula_weight         166.86

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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   6.12026(13)
_cell_length_b                   11.2342(2)
_cell_length_c                   8.55360(16)
_cell_angle_alpha                90
_cell_angle_beta                 96.8027(19)
_cell_angle_gamma                90
_cell_volume                     583.97(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    170.0(1)
_cell_measurement_reflns_used    6039
_cell_measurement_theta_min      1.80
_cell_measurement_theta_max      31.78

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.898
_exptl_crystal_F_000             312
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_exptl_absorpt_coefficient_mu    4.562
_shelx_estimated_absorpt_T_min   0.34
_shelx_estimated_absorpt_T_max   0.34
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.47
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?


# EXPERIMENTAL DATA

_exptl_special_details           
; 
Data were collected for the in-situ low-temperature crystallized
single crystal. 
;
_diffrn_ambient_temperature      170.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 8.0951
_diffrn_reflns_number            7680
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.812
_diffrn_reflns_theta_max         25.995
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             1139
_reflns_number_gt                1097
_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 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_cell_refinement       
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_data_reduction        
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury (Macrae at al., 2020)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

# REFINEMENT DATA 

_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)+(0.0152P)²+0.1475P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0072(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1139
_refine_ls_number_parameters     41
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0159
_refine_ls_R_factor_gt           0.0146
_refine_ls_wR_factor_ref         0.0348
_refine_ls_wR_factor_gt          0.0341
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_restrained_S_all      1.103
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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 0.48024(2) 0.33814(2) 0.42214(2) 0.03997(9) Uani 1 1 d . . . . .
C1 C 0.5212(4) 0.4134(2) 0.1975(3) 0.0521(6) Uani 1 1 d . . . . .
H11 H 0.4896 0.4971 0.1985 0.078 Uiso 1 1 calc R U . . .
H12 H 0.4224 0.3753 0.1174 0.078 Uiso 1 1 calc R U . . .
H13 H 0.6701 0.4017 0.1759 0.078 Uiso 1 1 calc R U . . .
C2 C 0.1279(4) 0.3460(2) 0.3847(4) 0.0573(7) Uani 1 1 d . . . . .
H21 H 0.0772 0.3174 0.2809 0.086 Uiso 1 1 calc R U . . .
H22 H 0.0807 0.4268 0.3950 0.086 Uiso 1 1 calc R U . . .
H23 H 0.0680 0.2973 0.4614 0.086 Uiso 1 1 calc R U . . .
C3 C 0.5003(5) 0.1569(2) 0.3470(4) 0.0569(7) Uani 1 1 d . . . . .
H31 H 0.6478 0.1398 0.3262 0.085 Uiso 1 1 calc R U . . .
H32 H 0.4008 0.1447 0.2529 0.085 Uiso 1 1 calc R U . . .
H33 H 0.4612 0.1048 0.4283 0.085 Uiso 1 1 calc R U . . .


# MOLECULAR GEOMETRY

_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 C1 2.141(2) . ?
Sb1 C3 2.143(2) . ?
Sb1 C2 2.144(3) . ?
C1 H11 0.9600 . ?
C1 H12 0.9600 . ?
C1 H13 0.9600 . ?
C2 H21 0.9600 . ?
C2 H22 0.9600 . ?
C2 H23 0.9600 . ?
C3 H31 0.9600 . ?
C3 H32 0.9600 . ?
C3 H33 0.9600 . ?

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
C1 Sb1 C3 95.13(11) . . ?
C1 Sb1 C2 94.14(10) . . ?
C3 Sb1 C2 94.97(11) . . ?
Sb1 C1 H11 109.5 . . ?
Sb1 C1 H12 109.5 . . ?
H11 C1 H12 109.5 . . ?
Sb1 C1 H13 109.5 . . ?
H11 C1 H13 109.5 . . ?
H12 C1 H13 109.5 . . ?
Sb1 C2 H21 109.5 . . ?
Sb1 C2 H22 109.5 . . ?
H21 C2 H22 109.5 . . ?
Sb1 C2 H23 109.5 . . ?
H21 C2 H23 109.5 . . ?
H22 C2 H23 109.5 . . ?
Sb1 C3 H31 109.5 . . ?
Sb1 C3 H32 109.5 . . ?
H31 C3 H32 109.5 . . ?
Sb1 C3 H33 109.5 . . ?
H31 C3 H33 109.5 . . ?
H32 C3 H33 109.5 . . ?

_refine_diff_density_max         0.354
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.053


####################################################################### 
# 
# 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_Me3As_C6F5I_180K
_database_code_depnum_ccdc_archive 'CCDC 2057070'
_audit_update_record             
;
2021-01-18 deposited with the CCDC.	2021-12-01 downloaded from the CCDC.
;

# CHEMICAL DATA

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H9 As, C6 F5 I'
_chemical_formula_sum            'C9 H9 As F5 I'
_chemical_formula_weight         413.98

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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_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                   11.5215(3)
_cell_length_b                   11.6259(3)
_cell_length_c                   20.0623(5)
_cell_angle_alpha                90
_cell_angle_beta                 102.807(3)
_cell_angle_gamma                90
_cell_volume                     2620.45(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    180.0(1)
_cell_measurement_reflns_used    8994
_cell_measurement_theta_min      2.08
_cell_measurement_theta_max      29.04

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.099
_exptl_crystal_F_000             1552
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    4.981
_shelx_estimated_absorpt_T_min   0.32
_shelx_estimated_absorpt_T_max   0.44
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.02
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?

# EXPERIMENTAL DATA

_exptl_special_details           
; 
Data were collected for the in-situ low-temperature cocrystallized
single crystal. 
;
_diffrn_ambient_temperature      180.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 8.0951
_diffrn_reflns_number            18126
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.082
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2574
_reflns_number_gt                2345
_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 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_cell_refinement       
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_data_reduction        
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury (Macrae at al., 2020)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

# REFINEMENT DATA 

_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)+(0.0301P)²+3.1412P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00064(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2574
_refine_ls_number_parameters     149
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0245
_refine_ls_wR_factor_ref         0.0628
_refine_ls_wR_factor_gt          0.0611
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.402
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.20789(3) 0.56346(3) 0.26025(2) 0.05917(13) Uani 1 1 d . . . . .
C1 C 0.3186(5) 0.4980(5) 0.2111(3) 0.1005(15) Uani 1 1 d . . . . .
H11 H 0.3642 0.5585 0.1966 0.151 Uiso 1 1 calc R U . . .
H12 H 0.2754 0.4572 0.1718 0.151 Uiso 1 1 calc R U . . .
H13 H 0.3712 0.4460 0.2404 0.151 Uiso 1 1 calc R U . . .
C2 C 0.3171(5) 0.6669(4) 0.3187(2) 0.0897(15) Uani 1 1 d . . . . .
H21 H 0.2735 0.7163 0.3427 0.134 Uiso 1 1 calc R U . . .
H22 H 0.3579 0.7127 0.2913 0.134 Uiso 1 1 calc R U . . .
H23 H 0.3739 0.6230 0.3510 0.134 Uiso 1 1 calc R U . . .
C3 C 0.1306(4) 0.6736(4) 0.1917(2) 0.0772(11) Uani 1 1 d . . . . .
H31 H 0.1899 0.7176 0.1761 0.116 Uiso 1 1 calc R U . . .
H32 H 0.0815 0.7244 0.2113 0.116 Uiso 1 1 calc R U . . .
H33 H 0.0821 0.6333 0.1538 0.116 Uiso 1 1 calc R U . . .
I1 I 0.09343(2) 0.39732(2) 0.36590(2) 0.05307(11) Uani 1 1 d . . . . .
C4 C 0.0402(3) 0.3050(3) 0.44375(15) 0.0494(7) Uani 1 1 d . . . . .
F1 F 0.1839(2) 0.16109(19) 0.44228(12) 0.0763(6) Uani 1 1 d . . . . .
C5 C 0.0948(3) 0.2030(3) 0.46820(17) 0.0583(9) Uani 1 1 d . . . . .
F2 F 0.1139(3) 0.0428(2) 0.54133(14) 0.1036(9) Uani 1 1 d . U . . .
C6 C 0.0611(4) 0.1421(4) 0.5193(2) 0.0771(13) Uani 1 1 d . . . . .
F3 F -0.0653(3) 0.1240(3) 0.59610(15) 0.1200(10) Uani 1 1 d . U . . .
C7 C -0.0306(5) 0.1846(5) 0.54635(19) 0.0914(17) Uani 1 1 d . . . . .
F4 F -0.1761(3) 0.3246(3) 0.54961(14) 0.1123(10) Uani 1 1 d . U . . .
C8 C -0.0864(4) 0.2852(5) 0.5232(2) 0.0798(13) Uani 1 1 d . . . . .
F5 F -0.1071(2) 0.4426(2) 0.45068(13) 0.0799(6) Uani 1 1 d . . . . .
C9 C -0.0510(3) 0.3450(3) 0.47193(18) 0.0614(9) Uani 1 1 d . . . . .


# MOLECULAR GEOMETRY

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As1 C1 1.933(5) . ?
As1 C2 1.936(4) . ?
As1 C3 1.945(4) . ?
C1 H11 0.9600 . ?
C1 H12 0.9600 . ?
C1 H13 0.9600 . ?
C2 H21 0.9600 . ?
C2 H22 0.9600 . ?
C2 H23 0.9600 . ?
C3 H31 0.9600 . ?
C3 H32 0.9600 . ?
C3 H33 0.9600 . ?
I1 C4 2.096(3) . ?
C4 C9 1.380(5) . ?
C4 C5 1.381(5) . ?
F1 C5 1.341(4) . ?
C5 C6 1.371(5) . ?
F2 C6 1.334(5) . ?
C6 C7 1.382(7) . ?
F3 C7 1.352(5) . ?
C7 C8 1.366(8) . ?
F4 C8 1.343(5) . ?
C8 C9 1.375(6) . ?
F5 C9 1.328(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 As1 C2 98.0(2) . . ?
C1 As1 C3 98.6(2) . . ?
C2 As1 C3 98.8(2) . . ?
As1 C1 H11 109.5 . . ?
As1 C1 H12 109.5 . . ?
H11 C1 H12 109.5 . . ?
As1 C1 H13 109.5 . . ?
H11 C1 H13 109.5 . . ?
H12 C1 H13 109.5 . . ?
As1 C2 H21 109.5 . . ?
As1 C2 H22 109.5 . . ?
H21 C2 H22 109.5 . . ?
As1 C2 H23 109.5 . . ?
H21 C2 H23 109.5 . . ?
H22 C2 H23 109.5 . . ?
As1 C3 H31 109.5 . . ?
As1 C3 H32 109.5 . . ?
H31 C3 H32 109.5 . . ?
As1 C3 H33 109.5 . . ?
H31 C3 H33 109.5 . . ?
H32 C3 H33 109.5 . . ?
C9 C4 C5 118.2(3) . . ?
C9 C4 I1 120.5(3) . . ?
C5 C4 I1 121.3(3) . . ?
F1 C5 C6 118.1(4) . . ?
F1 C5 C4 120.1(3) . . ?
C6 C5 C4 121.8(4) . . ?
F2 C6 C5 120.7(5) . . ?
F2 C6 C7 120.8(4) . . ?
C5 C6 C7 118.5(4) . . ?
F3 C7 C8 120.3(6) . . ?
F3 C7 C6 118.7(6) . . ?
C8 C7 C6 121.0(4) . . ?
F4 C8 C7 120.1(4) . . ?
F4 C8 C9 120.3(5) . . ?
C7 C8 C9 119.5(4) . . ?
F5 C9 C8 117.9(4) . . ?
F5 C9 C4 121.1(3) . . ?
C8 C9 C4 121.0(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 C4 C5 F1 -179.9(3) . . . . ?
I1 C4 C5 F1 0.1(4) . . . . ?
C9 C4 C5 C6 -0.3(5) . . . . ?
I1 C4 C5 C6 179.7(2) . . . . ?
F1 C5 C6 F2 -1.5(5) . . . . ?
C4 C5 C6 F2 178.9(3) . . . . ?
F1 C5 C6 C7 180.0(3) . . . . ?
C4 C5 C6 C7 0.4(5) . . . . ?
F2 C6 C7 F3 0.6(6) . . . . ?
C5 C6 C7 F3 179.1(3) . . . . ?
F2 C6 C7 C8 -178.8(3) . . . . ?
C5 C6 C7 C8 -0.3(6) . . . . ?
F3 C7 C8 F4 -0.1(6) . . . . ?
C6 C7 C8 F4 179.3(3) . . . . ?
F3 C7 C8 C9 -179.2(3) . . . . ?
C6 C7 C8 C9 0.2(6) . . . . ?
F4 C8 C9 F5 1.0(5) . . . . ?
C7 C8 C9 F5 -179.9(3) . . . . ?
F4 C8 C9 C4 -179.3(3) . . . . ?
C7 C8 C9 C4 -0.2(6) . . . . ?
C5 C4 C9 F5 179.9(3) . . . . ?
I1 C4 C9 F5 -0.1(4) . . . . ?
C5 C4 C9 C8 0.2(5) . . . . ?
I1 C4 C9 C8 -179.8(3) . . . . ?

_refine_diff_density_max         0.607
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.066


####################################################################### 
# 
# 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_Me3Sb_C6F5I_210K
_database_code_depnum_ccdc_archive 'CCDC 2057073'
_audit_update_record             
;
2021-01-18 deposited with the CCDC.	2021-12-01 downloaded from the CCDC.
;

# CHEMICAL DATA

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H9 Sb, C6 F5 I'
_chemical_formula_sum            'C9 H9 F5 I Sb'
_chemical_formula_weight         460.82

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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

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

_cell_length_a                   20.2334(16)
_cell_length_b                   6.0804(4)
_cell_length_c                   23.4856(16)
_cell_angle_alpha                90
_cell_angle_beta                 107.930(8)
_cell_angle_gamma                90
_cell_volume                     2749.0(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    210.0(1)
_cell_measurement_reflns_used    7276
_cell_measurement_theta_min      2.03
_cell_measurement_theta_max      30.02

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.227
_exptl_crystal_F_000             1696
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    4.283
_shelx_estimated_absorpt_T_min   0.67
_shelx_estimated_absorpt_T_max   0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.24
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?


# EXPERIMENTAL DATA

_exptl_special_details           
; 
Data were collected for the in-situ low-temperature cocrystallized
single crystal. 
;
_diffrn_ambient_temperature      210.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 8.0951
_diffrn_reflns_number            18500
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.823
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2714
_reflns_number_gt                2363
_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 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_cell_refinement       
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_data_reduction        
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury (Macrae at al., 2020)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

# REFINEMENT DATA 

_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)+(0.0277P)²+3.1968P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00097(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2714
_refine_ls_number_parameters     149
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0273
_refine_ls_wR_factor_ref         0.0663
_refine_ls_wR_factor_gt          0.0636
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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 0.27279(2) 0.40881(5) 0.39555(2) 0.06165(13) Uani 1 1 d . . . . .
C1 C 0.1847(4) 0.2010(11) 0.3817(4) 0.135(3) Uani 1 1 d . U . . .
H11 H 0.1733 0.1359 0.3426 0.203 Uiso 1 1 calc R U . . .
H12 H 0.1459 0.2861 0.3847 0.203 Uiso 1 1 calc R U . . .
H13 H 0.1950 0.0871 0.4115 0.203 Uiso 1 1 calc R U . . .
C2 C 0.3323(3) 0.1826(9) 0.3620(3) 0.0818(14) Uani 1 1 d . . . . .
H21 H 0.3707 0.2582 0.3550 0.123 Uiso 1 1 calc R U . . .
H22 H 0.3035 0.1205 0.3251 0.123 Uiso 1 1 calc R U . . .
H23 H 0.3494 0.0674 0.3906 0.123 Uiso 1 1 calc R U . . .
C3 C 0.2305(4) 0.5823(10) 0.3153(3) 0.120(2) Uani 1 1 d . . . . .
H31 H 0.2045 0.4832 0.2848 0.179 Uiso 1 1 calc R U . . .
H32 H 0.2674 0.6470 0.3031 0.179 Uiso 1 1 calc R U . . .
H33 H 0.2004 0.6961 0.3212 0.179 Uiso 1 1 calc R U . . .
I1 I 0.37485(2) 0.73732(4) 0.51514(2) 0.05557(12) Uani 1 1 d . . . . .
C4 C 0.4462(2) 0.9272(6) 0.58015(16) 0.0453(8) Uani 1 1 d . . . . .
F1 F 0.44725(15) 0.6697(4) 0.65556(11) 0.0714(7) Uani 1 1 d . . . . .
C5 C 0.4693(2) 0.8605(6) 0.63901(17) 0.0510(9) Uani 1 1 d . . . . .
F2 F 0.53852(17) 0.9105(5) 0.73892(11) 0.0881(9) Uani 1 1 d . . . . .
C6 C 0.5155(2) 0.9827(7) 0.68227(17) 0.0585(10) Uani 1 1 d . . . . .
F3 F 0.58410(15) 1.3010(5) 0.70823(12) 0.0837(8) Uani 1 1 d . . . . .
C7 C 0.5390(2) 1.1782(7) 0.6667(2) 0.0593(11) Uani 1 1 d . . . . .
F4 F 0.54016(15) 1.4411(4) 0.59384(13) 0.0743(7) Uani 1 1 d . . . . .
C8 C 0.5168(2) 1.2495(6) 0.6083(2) 0.0544(10) Uani 1 1 d . . . . .
F5 F 0.45095(14) 1.1950(4) 0.50938(10) 0.0646(6) Uani 1 1 d . . . . .
C9 C 0.4710(2) 1.1226(6) 0.56578(17) 0.0471(9) Uani 1 1 d . . . . .


# MOLECULAR GEOMETRY

_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 C3 2.099(6) . ?
Sb1 C1 2.127(6) . ?
Sb1 C2 2.132(5) . ?
C1 H11 0.9600 . ?
C1 H12 0.9600 . ?
C1 H13 0.9600 . ?
C2 H21 0.9600 . ?
C2 H22 0.9600 . ?
C2 H23 0.9600 . ?
C3 H31 0.9600 . ?
C3 H32 0.9600 . ?
C3 H33 0.9600 . ?
I1 C4 2.096(4) . ?
C4 C9 1.372(5) . ?
C4 C5 1.377(5) . ?
F1 C5 1.343(5) . ?
C5 C6 1.369(6) . ?
F2 C6 1.341(5) . ?
C6 C7 1.370(7) . ?
F3 C7 1.339(5) . ?
C7 C8 1.377(6) . ?
F4 C8 1.339(5) . ?
C8 C9 1.371(5) . ?
F5 C9 1.335(4) . ?

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
C3 Sb1 C1 94.0(3) . . ?
C3 Sb1 C2 96.4(3) . . ?
C1 Sb1 C2 95.9(2) . . ?
Sb1 C1 H11 109.5 . . ?
Sb1 C1 H12 109.5 . . ?
H11 C1 H12 109.5 . . ?
Sb1 C1 H13 109.5 . . ?
H11 C1 H13 109.5 . . ?
H12 C1 H13 109.5 . . ?
Sb1 C2 H21 109.5 . . ?
Sb1 C2 H22 109.5 . . ?
H21 C2 H22 109.5 . . ?
Sb1 C2 H23 109.5 . . ?
H21 C2 H23 109.5 . . ?
H22 C2 H23 109.5 . . ?
Sb1 C3 H31 109.5 . . ?
Sb1 C3 H32 109.5 . . ?
H31 C3 H32 109.5 . . ?
Sb1 C3 H33 109.5 . . ?
H31 C3 H33 109.5 . . ?
H32 C3 H33 109.5 . . ?
C9 C4 C5 117.7(3) . . ?
C9 C4 I1 121.3(3) . . ?
C5 C4 I1 120.9(3) . . ?
F1 C5 C6 117.8(3) . . ?
F1 C5 C4 120.3(3) . . ?
C6 C5 C4 121.9(4) . . ?
F2 C6 C5 120.5(4) . . ?
F2 C6 C7 120.4(4) . . ?
C5 C6 C7 119.1(4) . . ?
F3 C7 C6 120.3(4) . . ?
F3 C7 C8 119.3(4) . . ?
C6 C7 C8 120.4(4) . . ?
F4 C8 C9 121.2(4) . . ?
F4 C8 C7 119.6(4) . . ?
C9 C8 C7 119.2(4) . . ?
F5 C9 C8 117.8(3) . . ?
F5 C9 C4 120.5(3) . . ?
C8 C9 C4 121.7(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 C4 C5 F1 -179.4(3) . . . . ?
I1 C4 C5 F1 1.2(5) . . . . ?
C9 C4 C5 C6 -0.1(6) . . . . ?
I1 C4 C5 C6 -179.5(3) . . . . ?
F1 C5 C6 F2 1.1(6) . . . . ?
C4 C5 C6 F2 -178.1(4) . . . . ?
F1 C5 C6 C7 180.0(4) . . . . ?
C4 C5 C6 C7 0.7(6) . . . . ?
F2 C6 C7 F3 -1.2(6) . . . . ?
C5 C6 C7 F3 179.9(4) . . . . ?
F2 C6 C7 C8 178.3(4) . . . . ?
C5 C6 C7 C8 -0.6(6) . . . . ?
F3 C7 C8 F4 -0.5(6) . . . . ?
C6 C7 C8 F4 180.0(4) . . . . ?
F3 C7 C8 C9 179.5(4) . . . . ?
C6 C7 C8 C9 0.0(6) . . . . ?
F4 C8 C9 F5 0.6(5) . . . . ?
C7 C8 C9 F5 -179.4(4) . . . . ?
F4 C8 C9 C4 -179.4(3) . . . . ?
C7 C8 C9 C4 0.6(6) . . . . ?
C5 C4 C9 F5 179.5(3) . . . . ?
I1 C4 C9 F5 -1.1(5) . . . . ?
C5 C4 C9 C8 -0.5(6) . . . . ?
I1 C4 C9 C8 178.8(3) . . . . ?

_refine_diff_density_max         0.920
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.084



_vrf_PLAT242_Me3Sb_C6F5I_210K    
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Sb1 Check        
 
RESPONSE: The assignment of Sb atom is correct. This is a false alert
associated with the presence of the terminal methyl groups.
;
####################################################################### 
# 
# 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_Me3Sb_150K
_database_code_depnum_ccdc_archive 'CCDC 2057067'
_audit_update_record             
;
2021-01-18 deposited with the CCDC.	2021-12-01 downloaded from the CCDC.
;

# CHEMICAL DATA

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H9 Sb'
_chemical_formula_sum            'C3 H9 Sb'
_chemical_formula_weight         166.86

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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   6.09729(11)
_cell_length_b                   11.20824(19)
_cell_length_c                   8.52671(15)
_cell_angle_alpha                90
_cell_angle_beta                 96.7940(17)
_cell_angle_gamma                90
_cell_volume                     578.623(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.0(1)
_cell_measurement_reflns_used    6510
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      31.89

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.916
_exptl_crystal_F_000             312
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_exptl_absorpt_coefficient_mu    4.604
_shelx_estimated_absorpt_T_min   0.34
_shelx_estimated_absorpt_T_max   0.34
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.46
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?


# EXPERIMENTAL DATA

_exptl_special_details           
; 
Data were collected for the in-situ low-temperature crystallized
single crystal. 
;
_diffrn_ambient_temperature      150.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 8.0951
_diffrn_reflns_number            7596
_diffrn_reflns_av_unetI/netI     0.0132
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.015
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             1128
_reflns_number_gt                1090
_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 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_cell_refinement       
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_data_reduction        
'CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury (Macrae at al., 2020)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

# REFINEMENT DATA 

_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)+(0.0106P)²+0.2464P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0116(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1128
_refine_ls_number_parameters     41
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0145
_refine_ls_R_factor_gt           0.0134
_refine_ls_wR_factor_ref         0.0294
_refine_ls_wR_factor_gt          0.0290
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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 0.47936(2) 0.33837(2) 0.42172(2) 0.03378(8) Uani 1 1 d . . . . .
C1 C 0.5190(4) 0.4142(2) 0.1961(3) 0.0444(5) Uani 1 1 d . . . . .
H11 H 0.4875 0.4981 0.1975 0.067 Uiso 1 1 calc R U . . .
H12 H 0.4191 0.3761 0.1159 0.067 Uiso 1 1 calc R U . . .
H13 H 0.6682 0.4024 0.1737 0.067 Uiso 1 1 calc R U . . .
C2 C 0.1252(4) 0.3457(2) 0.3847(3) 0.0498(6) Uani 1 1 d . . . . .
H21 H 0.0738 0.3117 0.2837 0.075 Uiso 1 1 calc R U . . .
H22 H 0.0779 0.4273 0.3876 0.075 Uiso 1 1 calc R U . . .
H23 H 0.0658 0.3014 0.4663 0.075 Uiso 1 1 calc R U . . .
C3 C 0.4998(4) 0.15639(19) 0.3459(3) 0.0487(6) Uani 1 1 d . . . . .
H31 H 0.6480 0.1393 0.3254 0.073 Uiso 1 1 calc R U . . .
H32 H 0.4004 0.1443 0.2513 0.073 Uiso 1 1 calc R U . . .
H33 H 0.4600 0.1042 0.4272 0.073 Uiso 1 1 calc R U . . .


# MOLECULAR GEOMETRY

_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 C1 2.143(2) . ?
Sb1 C2 2.146(2) . ?
Sb1 C3 2.148(2) . ?
C1 H11 0.9600 . ?
C1 H12 0.9600 . ?
C1 H13 0.9600 . ?
C2 H21 0.9600 . ?
C2 H22 0.9600 . ?
C2 H23 0.9600 . ?
C3 H31 0.9600 . ?
C3 H32 0.9600 . ?
C3 H33 0.9600 . ?

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
C1 Sb1 C2 94.08(9) . . ?
C1 Sb1 C3 95.15(10) . . ?
C2 Sb1 C3 94.89(10) . . ?
Sb1 C1 H11 109.5 . . ?
Sb1 C1 H12 109.5 . . ?
H11 C1 H12 109.5 . . ?
Sb1 C1 H13 109.5 . . ?
H11 C1 H13 109.5 . . ?
H12 C1 H13 109.5 . . ?
Sb1 C2 H21 109.5 . . ?
Sb1 C2 H22 109.5 . . ?
H21 C2 H22 109.5 . . ?
Sb1 C2 H23 109.5 . . ?
H21 C2 H23 109.5 . . ?
H22 C2 H23 109.5 . . ?
Sb1 C3 H31 109.5 . . ?
Sb1 C3 H32 109.5 . . ?
H31 C3 H32 109.5 . . ?
Sb1 C3 H33 109.5 . . ?
H31 C3 H33 109.5 . . ?
H32 C3 H33 109.5 . . ?

_refine_diff_density_max         0.447
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.051


