# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_Ti
_database_code_depnum_ccdc_archive 'CCDC 2141584'
loop_
_audit_author_name
_audit_author_address
'Jiang Long'
;Sun Yat Sen Universit
China
;
_audit_update_record             
;
2022-01-12 deposited with the CCDC.	2022-02-22 downloaded from the CCDC.
;
_audit_creation_date             2021-06-18
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'F6 Ti, 2(C4 H12 N1)'
_chemical_formula_sum            'C8 H24 F6 N2 Ti'
_chemical_formula_weight         310.18
_chemical_melting_point          ?
_chemical_oxdiff_usercomment     ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   7.8913(2)
_cell_length_b                   7.8913(2)
_cell_length_c                   19.9262(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1074.61(7)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    6642
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      40.8970
_cell_measurement_theta_min      5.0560
_shelx_estimated_absorpt_T_max   0.981
_shelx_estimated_absorpt_T_min   0.950
_exptl_absorpt_coefficient_mu    0.646
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86983
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             486
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            7932
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         41.281
_diffrn_reflns_theta_min         5.064
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -40.00   8.00   1.00   30.00    --  -38.85  38.00-180.00   48
  2  ω   -125.00 -70.00   1.00   30.00    --  -38.85 178.00 150.00   55
  3  ω     20.00 114.00   1.00   30.00    --   40.10  38.00   0.00   94
  4  ω     35.00 109.00   1.00   30.00    --   40.10 178.00 -60.00   74
  5  ω    -32.00  -1.00   1.00   30.00    --   40.10 -57.00 -90.00   31
  6  ω      1.00  81.00   1.00   30.00    --   40.10 -99.00 120.00   80
  7  ω      8.00 114.00   1.00   30.00    --   40.10  77.00  30.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0862956000
_diffrn_orient_matrix_UB_12      -0.0124638000
_diffrn_orient_matrix_UB_13      -0.0156011000
_diffrn_orient_matrix_UB_21      -0.0521993000
_diffrn_orient_matrix_UB_22      -0.0374514000
_diffrn_orient_matrix_UB_23      0.0304340000
_diffrn_orient_matrix_UB_31      0.0245469000
_diffrn_orient_matrix_UB_32      0.0960062000
_diffrn_orient_matrix_UB_33      0.0098465000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1561
_reflns_number_total             1578
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     40.15
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     30
_refine_ls_number_reflns         1578
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0241
_refine_ls_restrained_S_all      1.124
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0381P)²+0.0474P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0674
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.91698
 0.08302
2. Others
 Fixed Sof: H1B(0.3333) H1C(0.3333) H1A(0.3333)
3.a Idealised Me refined as rotating group:
 C1(H1B,H1C,H1A), C2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Ti1 Ti 0.0000 1.0000 0.5000 0.01298(5) Uani 1 6 d S T P . .
F1 F -0.05919(7) 0.78457(7) 0.44611(2) 0.02575(9) Uani 1 1 d . . . . .
N1 N 0.3333 0.6667 0.41380(4) 0.01465(10) Uani 1 3 d S T P . .
C1 C 0.3333 0.6667 0.48880(5) 0.02407(17) Uani 1 3 d S T P . .
H1B H 0.4643 0.7494 0.5049 0.036 Uiso 0.3333 1 calc GR . . A -1
H1C H 0.2851 0.5357 0.5049 0.036 Uiso 0.3333 1 calc GR . . A -1
H1A H 0.2506 0.7149 0.5049 0.036 Uiso 0.3333 1 calc GR . . A -1
C2 C 0.39647(10) 0.86830(9) 0.38890(3) 0.02157(10) Uani 1 1 d . . . . .
H2A H 0.3099 0.9104 0.4061 0.032 Uiso 1 1 calc GR . . . .
H2B H 0.3926 0.8677 0.3407 0.032 Uiso 1 1 calc GR . . . .
H2C H 0.5274 0.9564 0.4038 0.032 Uiso 1 1 calc GR . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ti1 0.01328(6) 0.01328(6) 0.01240(8) 0.000 0.000 0.00664(3)
F1 0.02876(19) 0.02193(17) 0.02675(19) -0.00916(14) -0.00213(14) 0.01280(15)
N1 0.01472(15) 0.01472(15) 0.0145(2) 0.000 0.000 0.00736(7)
C1 0.0289(3) 0.0289(3) 0.0143(3) 0.000 0.000 0.01447(13)
C2 0.0221(2) 0.01629(19) 0.0260(2) 0.00389(17) 0.00163(17) 0.00935(17)

_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
Ti1 F1 1.8621(4) . ?
Ti1 F1 1.8621(4) 2_675 ?
Ti1 F1 1.8621(4) 10_576 ?
Ti1 F1 1.8621(4) 11_456 ?
Ti1 F1 1.8621(4) 3_465 ?
Ti1 F1 1.8621(4) 12_666 ?
N1 C1 1.4946(12) . ?
N1 C2 1.4944(6) 3_565 ?
N1 C2 1.4944(6) 2_665 ?
N1 C2 1.4944(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F1 Ti1 F1 180.0 . 10_576 ?
F1 Ti1 F1 90.06(2) 3_465 2_675 ?
F1 Ti1 F1 90.06(2) . 2_675 ?
F1 Ti1 F1 89.94(2) 12_666 2_675 ?
F1 Ti1 F1 180.0 12_666 3_465 ?
F1 Ti1 F1 89.94(2) 3_465 11_456 ?
F1 Ti1 F1 90.06(2) . 3_465 ?
F1 Ti1 F1 89.94(2) . 12_666 ?
F1 Ti1 F1 89.94(2) 10_576 3_465 ?
F1 Ti1 F1 90.06(2) 10_576 11_456 ?
F1 Ti1 F1 180.0 2_675 11_456 ?
F1 Ti1 F1 90.06(2) 10_576 12_666 ?
F1 Ti1 F1 89.94(2) . 11_456 ?
F1 Ti1 F1 89.94(2) 10_576 2_675 ?
F1 Ti1 F1 90.06(2) 12_666 11_456 ?
C1 N1 C2 109.38(4) . 3_565 ?
C2 N1 C1 109.38(4) . . ?
C2 N1 C1 109.38(4) 2_665 . ?
C2 N1 C2 109.56(4) . 3_565 ?
C2 N1 C2 109.56(4) 2_665 3_565 ?
C2 N1 C2 109.56(4) . 2_665 ?

_iucr_refine_instructions_details 
;
    Ti.res created by SHELXL-2014/7

TITL Ti.res in R-3
REM Ti.res in R-3
REM SHELXT solution in R-3
REM R1 0.146, Rweak 0.063, Alpha 0.094, Orientation as input
REM Formula found by SHELXT: C1 F14 Mn
CELL 0.71073 7.8913 7.8913 19.9262 90 90 120
ZERR 3.00006 0.0002 0.0002 0.0007 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SFAC C H F N Ti
UNIT 24 72 18 6 3
 
L.S. 5 0 0
PLAN  20
SIZE 0.03 0.05 0.08
list 4
fmap 2 53
ACTA
TWIN 0 1 0 1 0 0 0 0 -1 2
OMIT 0 1 2
OMIT -3 3 6
OMIT 0 0 12
REM <olex2.extras>
REM <HklSrc "%.\\Ti.hkl">
REM </olex2.extras>
 
WGHT    0.038100    0.047400
BASF   0.08302
FVAR       0.74078
TI1   5    0.000000    1.000000    0.500000    10.16667    0.01328    0.01328 =
         0.01240    0.00000    0.00000    0.00664
F1    3   -0.059188    0.784573    0.446107    11.00000    0.02876    0.02193 =
         0.02675   -0.00916   -0.00213    0.01280
N1    4    0.333333    0.666667    0.413796    10.33333    0.01472    0.01472 =
         0.01451    0.00000    0.00000    0.00736
C1    1    0.333333    0.666667    0.488802    10.33333    0.02893    0.02893 =
         0.01435    0.00000    0.00000    0.01447
PART -1
AFIX 137
H1B   2    0.464272    0.749353    0.504861    10.33333   -1.50000
H1C   2    0.285082    0.535728    0.504861    10.33333   -1.50000
H1A   2    0.250647    0.714918    0.504861    10.33333   -1.50000
AFIX   0
PART 0
C2    1    0.396472    0.868303    0.388904    11.00000    0.02210    0.01629 =
         0.02598    0.00389    0.00163    0.00935
AFIX 137
H2A   2    0.309895    0.910361    0.406138    11.00000   -1.50000
H2B   2    0.392633    0.867666    0.340747    11.00000   -1.50000
H2C   2    0.527448    0.956413    0.403836    11.00000   -1.50000
AFIX   0
HKLF 4
 
REM  Ti.res in R-3
REM R1 =  0.0241 for    1561 Fo > 4sig(Fo)  and  0.0244 for all    1578 data
REM     30 parameters refined using      0 restraints
 
END  
     
WGHT      0.0381      0.0474 

REM Highest difference peak  0.331,  deepest hole -0.453,  1-sigma level  0.051
Q1    1  -0.0478  0.8853  0.4670  11.00000  0.05    0.33
Q2    1   0.3576  0.7412  0.3999  11.00000  0.05    0.32
Q3    1   0.3333  0.6667  0.4464  10.33333  0.05    0.32
Q4    1   0.0000  1.0000  0.4646  10.33333  0.05    0.22
Q5    1  -0.0202  0.8575  0.4262  11.00000  0.05    0.21
Q6    1  -0.1319  0.7543  0.4656  11.00000  0.05    0.21
Q7    1   0.0151  0.9008  0.4621  11.00000  0.05    0.18
Q8    1   0.6667  1.3333  0.3333  10.16667  0.05    0.17
Q9    1  -0.0605  0.7438  0.4854  11.00000  0.05    0.17
Q10   1  -0.1259  0.8233  0.4258  11.00000  0.05    0.15
Q11   1   0.0227  0.9018  0.4106  11.00000  0.05    0.15
Q12   1   0.3469  0.8141  0.2882  11.00000  0.05    0.14
Q13   1   0.4903  0.9178  0.4287  11.00000  0.05    0.13
Q14   1   0.4955  0.9854  0.4260  11.00000  0.05    0.13
Q15   1  -0.0354  0.9279  0.4320  11.00000  0.05    0.13
Q16   1  -0.0566  0.7683  0.3973  11.00000  0.05    0.13
Q17   1  -0.0830  0.7145  0.4280  11.00000  0.05    0.12
Q18   1  -0.0674  0.7990  0.4866  11.00000  0.05    0.12
Q19   1   0.0289  0.8402  0.4154  11.00000  0.05    0.12
Q20   1   0.2783  0.4557  0.5398  11.00000  0.05    0.12

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0241 for 1561 Fo > 4sig(Fo) and 0.0244 for all 7949 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.33, deepest hole -0.45
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0244
  REM R1_gt = 0.0241
  REM wR_ref = 0.0674
  REM GOOF = 1.124
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 7949
  REM Reflections_gt = 1561
  REM Parameters = n/a
  REM Hole = -0.45
  REM Peak = 0.33
  REM Flack = n/a
;
_olex2_date_sample_data_collection 2020-07-09
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.147
_oxdiff_exptl_absorpt_empirical_full_min 0.849
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.91698
2 0.08302

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
####################################################################### 
# 
# 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_Si
_database_code_depnum_ccdc_archive 'CCDC 2141586'
loop_
_audit_author_name
_audit_author_address
'Jiang Long'
;Sun Yat Sen Universit
China
;
_audit_update_record             
;
2022-01-12 deposited with the CCDC.	2022-02-22 downloaded from the CCDC.
;
_audit_creation_date             2021-06-18
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C4 H12 N1), F6 Si1'
_chemical_formula_sum            'C8 H24 F6 N2 Si'
_chemical_formula_weight         290.37
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNFSi
_chemical_oxdiff_usercomment     ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   7.7802(8)
_cell_length_b                   7.7802(8)
_cell_length_c                   19.544(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1024.5(2)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    577
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      71.9930
_cell_measurement_theta_min      6.9490
_shelx_estimated_absorpt_T_max   0.941
_shelx_estimated_absorpt_T_min   0.852
_exptl_absorpt_coefficient_mu    2.061
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38277
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             462
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            714
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.993
_diffrn_reflns_theta_min         6.796
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     29.00  70.00   1.00    1.29    --   41.14-125.00 120.00   41
  2  ω    104.00 133.00   1.00    5.17    --  105.29  77.00-180.00   29
  3  ω    134.00 178.00   1.00    5.17    --  105.29  77.00  30.00   44
  4  ω    -71.00  -9.00   1.00    1.29    --  -41.52 125.00 -90.00   62
  5  ω     30.00  62.00   1.00    5.17    --  105.29 -94.00 120.00   32
  6  ω     65.00 101.00   1.00    5.17    --  105.29 -94.00 120.00   36
  7  ω    134.00 160.00   1.00    5.17    --  105.29  77.00  60.00   26
  8  ω    101.00 177.00   1.00    5.17    --  105.29 125.00 120.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1818155333
_diffrn_orient_matrix_UB_12      -0.2020234667
_diffrn_orient_matrix_UB_13      0.0180051333
_diffrn_orient_matrix_UB_21      -0.0700246333
_diffrn_orient_matrix_UB_22      0.1034631333
_diffrn_orient_matrix_UB_23      0.0508878333
_diffrn_orient_matrix_UB_31      -0.1199179000
_diffrn_orient_matrix_UB_32      0.0277310000
_diffrn_orient_matrix_UB_33      -0.0573650000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                423
_reflns_number_total             434
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.141
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     30
_refine_ls_number_reflns         434
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0714
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1442P)²+0.6168P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1828
_refine_ls_wR_factor_ref         0.1829
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.10804
 0.89196
2. Others
 Fixed Sof: H2A(0.3333) H2B(0.3333) H2C(0.3333)
3.a Idealised Me refined as rotating group:
 C1(H1B,H1A,H1C), C2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
C1 C 0.4727(4) 0.8723(4) 0.38920(15) 0.0222(8) Uani 1 1 d . . . . .
H1B H 0.6042 0.9144 0.4056 0.033 Uiso 1 1 calc GR . . . .
H1A H 0.4303 0.9613 0.4057 0.033 Uiso 1 1 calc GR . . . .
H1C H 0.4728 0.8729 0.3401 0.033 Uiso 1 1 calc GR . . . .
C2 C 0.3333 0.6667 0.4913(2) 0.0249(11) Uani 1 3 d S T P . .
H2A H 0.2903 0.7553 0.5077 0.037 Uiso 0.3333 1 calc GR . . A -1
H2B H 0.4651 0.7097 0.5077 0.037 Uiso 0.3333 1 calc GR . . A -1
H2C H 0.2447 0.5349 0.5077 0.037 Uiso 0.3333 1 calc GR . . A -1
N1 N 0.3333 0.6667 0.41446(18) 0.0164(9) Uani 1 3 d S T P . .
F1 F 0.9490(3) 1.1467(3) 0.45009(9) 0.0266(7) Uani 1 1 d . . . . .
Si1 Si 1.0000 1.0000 0.5000 0.0131(6) Uani 1 6 d S T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0192(14) 0.0156(15) 0.0311(15) 0.0046(12) 0.0026(11) 0.0082(12)
C2 0.0290(16) 0.0290(16) 0.017(2) 0.000 0.000 0.0145(8)
N1 0.0158(12) 0.0158(12) 0.0176(17) 0.000 0.000 0.0079(6)
F1 0.0270(10) 0.0241(11) 0.0307(11) 0.0079(7) -0.0023(7) 0.0143(8)
Si1 0.0118(7) 0.0118(7) 0.0158(9) 0.000 0.000 0.0059(3)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1B 0.9600 . ?
C1 H1A 0.9600 . ?
C1 H1C 0.9600 . ?
C1 N1 1.498(3) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C2 N1 1.502(6) . ?
N1 C1 1.498(3) 2_665 ?
N1 C1 1.498(3) 3_565 ?
F1 Si1 1.6926(17) . ?
Si1 F1 1.6926(17) 2_765 ?
Si1 F1 1.6926(17) 3_675 ?
Si1 F1 1.6926(17) 12_656 ?
Si1 F1 1.6926(17) 10_776 ?
Si1 F1 1.6926(17) 11_566 ?

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
H1B C1 H1A 109.5 . . ?
H1B C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
C1 N1 C1 109.70(17) 2_665 3_565 ?
C1 N1 C1 109.70(17) . 2_665 ?
C1 N1 C1 109.70(17) . 3_565 ?
C1 N1 C2 109.25(17) . . ?
C1 N1 C2 109.25(17) 3_565 . ?
C1 N1 C2 109.25(17) 2_665 . ?
F1 Si1 F1 89.90(9) . 11_566 ?
F1 Si1 F1 89.90(9) 11_566 3_675 ?
F1 Si1 F1 90.10(9) 11_566 12_656 ?
F1 Si1 F1 90.10(9) . 3_675 ?
F1 Si1 F1 90.10(9) 2_765 3_675 ?
F1 Si1 F1 180.0 12_656 3_675 ?
F1 Si1 F1 89.90(9) 2_765 12_656 ?
F1 Si1 F1 90.10(9) 11_566 10_776 ?
F1 Si1 F1 89.90(9) 2_765 10_776 ?
F1 Si1 F1 180.0 11_566 2_765 ?
F1 Si1 F1 89.90(9) 10_776 3_675 ?
F1 Si1 F1 89.90(9) . 12_656 ?
F1 Si1 F1 180.0 . 10_776 ?
F1 Si1 F1 90.10(9) . 2_765 ?
F1 Si1 F1 90.10(9) 10_776 12_656 ?

_iucr_refine_instructions_details 
;
    exp_1792.res created by SHELXL-2014/7

TITL Si.res in R-3
REM Old TITL Si in R-3
REM SHELXT solution in R-3
REM R1 0.175, Rweak 0.064, Alpha 0.084, Orientation as input
REM Formula found by SHELXT: C8 N2 F6 Si
CELL 1.54184 7.78016 7.78016 19.543735 90 90 120
ZERR 3.00006 0.000752 0.000752 0.001979 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SFAC C H F N Si
UNIT 24 72 18 6 3
 
L.S. 4
PLAN  20
SIZE 0.03 0.04 0.08
BOND $H
list 4
fmap 2
acta
TWIN -1 -1 0 0 1 0 0 0 -1 2
OMIT 0 3 0
OMIT -2 6 4
OMIT -4 7 4
OMIT -4 6 8
OMIT 1 4 15
OMIT 2 4 16
OMIT -3 6 3
OMIT -3 6 6
OMIT -3 5 7
REM <olex2.extras>
REM <HklSrc "%.\\Si.hkl">
REM </olex2.extras>
 
WGHT    0.144200    0.616800
BASF   0.89196
FVAR       8.31624
C1    1    0.472655    0.872253    0.389202    11.00000    0.01918    0.01562 =
         0.03115    0.00456    0.00256    0.00815
AFIX 137
H1B   2    0.604168    0.914386    0.405595    11.00000   -1.50000
H1A   2    0.430261    0.961291    0.405739    11.00000   -1.50000
H1C   2    0.472836    0.872855    0.340082    11.00000   -1.50000
AFIX   0
C2    1    0.333333    0.666667    0.491339    10.33333    0.02901    0.02901 =
         0.01658    0.00000    0.00000    0.01451
PART -1
AFIX 137
H2A   2    0.290266    0.755326    0.507712    10.33333   -1.50000
H2B   2    0.465060    0.709734    0.507712    10.33333   -1.50000
H2C   2    0.244674    0.534940    0.507712    10.33333   -1.50000
AFIX   0
PART 0
N1    4    0.333333    0.666667    0.414463    10.33333    0.01577    0.01577 =
         0.01761    0.00000    0.00000    0.00789
F1    3    0.949018    1.146725    0.450088    11.00000    0.02696    0.02412 =
         0.03066    0.00786   -0.00233    0.01426
SI1   5    1.000000    1.000000    0.500000    10.16667    0.01176    0.01176 =
         0.01583    0.00000    0.00000    0.00588
HKLF 4
 
REM  Si.res in R-3
REM R1 =  0.0714 for     423 Fo > 4sig(Fo)  and  0.0716 for all     434 data
REM     30 parameters refined using      0 restraints
 
END  
     
WGHT      0.1445      0.8182 

REM Highest difference peak  0.767,  deepest hole -0.496,  1-sigma level  0.141
Q1    1   0.9530  1.0733  0.4719  11.00000  0.05    0.62
Q2    1   0.8247  1.0930  0.4733  11.00000  0.05    0.53
Q3    1   0.4054  0.9706  0.3594  11.00000  0.05    0.43
Q4    1   0.1931  0.4543  0.5194  11.00000  0.05    0.40
Q5    1   0.4621  0.8785  0.2787  11.00000  0.05    0.38
Q6    1   0.4216  0.9898  0.4412  11.00000  0.05    0.37
Q7    1   0.9393  1.1071  0.4185  11.00000  0.05    0.33
Q8    1   0.6533  0.8759  0.3702  11.00000  0.05    0.32
Q9    1   0.3333  0.6667  0.5648  10.33333  0.05    0.31
Q10   1   0.4898  0.5940  0.5374  11.00000  0.05    0.31
Q11   1   0.9144  1.1974  0.4196  11.00000  0.05    0.31
Q12   1   0.7027  1.2241  0.3761  11.00000  0.05    0.30
Q13   1   0.4163  0.8192  0.4350  11.00000  0.05    0.28
Q14   1   1.0012  1.2619  0.4514  11.00000  0.05    0.26
Q15   1   0.5059  0.8186  0.3033  11.00000  0.05    0.25
Q16   1   0.5434  0.8073  0.4032  11.00000  0.05    0.24
Q17   1   0.6266  1.0357  0.3818  11.00000  0.05    0.23
Q18   1   0.4812  1.1084  0.3736  11.00000  0.05    0.23
Q19   1   0.6212  1.2437  0.3375  11.00000  0.05    0.23
Q20   1   0.5926  0.8562  0.5396  11.00000  0.05    0.22

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0714 for 423 Fo > 4sig(Fo) and 0.0716 for all 727 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.77, deepest hole -0.50
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0716
  REM R1_gt = 0.0714
  REM wR_ref = 0.1829
  REM GOOF = 1.095
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 727
  REM Reflections_gt = 423
  REM Parameters = n/a
  REM Hole = -0.50
  REM Peak = 0.77
  REM Flack = n/a
;
_olex2_date_sample_data_collection 2021-06-08
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.380
_oxdiff_exptl_absorpt_empirical_full_min 0.624
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.10804
2 0.89196

####################################################################### 
# 
# 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_Ge
_database_code_depnum_ccdc_archive 'CCDC 2141588'
loop_
_audit_author_name
_audit_author_address
'Jiang Long'
;Sun Yat Sen Universit
China
;
_audit_update_record             
;
2022-01-12 deposited with the CCDC.	2022-02-22 downloaded from the CCDC.
;
_audit_creation_date             2021-06-18
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C4 H12 N1), F6 Ge'
_chemical_formula_sum            'C8 H24 F6 Ge N2'
_chemical_formula_weight         334.87
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNGeF
_chemical_oxdiff_usercomment     ?
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'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   7.8554(5)
_cell_length_b                   7.8554(5)
_cell_length_c                   19.6666(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1050.98(16)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    3014
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      36.5180
_cell_measurement_theta_min      5.1630
_shelx_estimated_absorpt_T_max   0.663
_shelx_estimated_absorpt_T_min   0.553
_exptl_absorpt_coefficient_mu    2.237
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0747
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            3570
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.716
_diffrn_reflns_theta_min         3.642
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -116.00 -90.00   1.00   15.00    --  -28.39-178.00 -30.00   26
  2  ω     38.00 112.00   1.00   15.00    --   29.33-178.00  30.00   74
  3  ω     61.00 104.00   1.00   15.00    --   29.33 159.00-134.00   43
  4  ω     34.00  89.00   1.00   15.00    --   29.33  38.00 -30.00   55
  5  ω      6.00  95.00   1.00   15.00    --   29.33  38.00-180.00   89
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1017170000
_diffrn_orient_matrix_UB_12      0.0668450000
_diffrn_orient_matrix_UB_13      -0.0045529000
_diffrn_orient_matrix_UB_21      -0.0107937000
_diffrn_orient_matrix_UB_22      0.0746310000
_diffrn_orient_matrix_UB_23      0.0163446000
_diffrn_orient_matrix_UB_31      0.0199731000
_diffrn_orient_matrix_UB_32      -0.0287881000
_diffrn_orient_matrix_UB_33      0.0318142000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1105
_reflns_number_total             1112
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     35.02
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.138
_refine_diff_density_min         -1.243
_refine_diff_density_rms         0.188
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     29
_refine_ls_number_reflns         1112
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0668
_refine_ls_restrained_S_all      1.149
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0753P)²+9.9390P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1734
_refine_ls_wR_factor_ref         0.1740
_refine_special_details          ?
_olex2_refinement_description    
;
1. Others
 Fixed Sof: H2B(0.3333) H2C(0.3333) H2A(0.3333)
2.a Idealised Me refined as rotating group:
 C1(H1B,H1C,H1A), C2(H2B,H2C,H2A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
C1 C 0.5368(5) 0.8029(6) 0.44378(18) 0.0285(7) Uani 1 1 d . . . . .
H1B H 0.6228 0.7561 0.4292 0.043 Uiso 1 1 calc GR . . . .
H1C H 0.5364 0.8084 0.4925 0.043 Uiso 1 1 calc GR . . . .
H1A H 0.5822 0.9320 0.4256 0.043 Uiso 1 1 calc GR . . . .
C2 C 0.3333 0.6667 0.3435(3) 0.0286(11) Uani 1 3 d S T P . .
H2B H 0.2016 0.5845 0.3273 0.043 Uiso 0.3333 1 calc GR . . A -1
H2C H 0.4155 0.6172 0.3273 0.043 Uiso 0.3333 1 calc GR . . A -1
H2A H 0.3828 0.7984 0.3273 0.043 Uiso 0.3333 1 calc GR . . A -1
N1 N 0.3333 0.6667 0.4189(2) 0.0148(6) Uani 1 3 d S T P . .
F1 F 0.4589(4) 1.1824(4) 0.38536(13) 0.0344(6) Uani 1 1 d . . . . .
Ge1 Ge 0.6667 1.3333 0.3333 0.0128(2) Uani 1 6 d S T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0187(13) 0.0324(16) 0.0286(14) -0.0021(12) -0.0053(11) 0.0085(12)
C2 0.0355(18) 0.0355(18) 0.0148(18) 0.000 0.000 0.0178(9)
N1 0.0138(9) 0.0138(9) 0.0170(14) 0.000 0.000 0.0069(4)
F1 0.0312(12) 0.0351(12) 0.0325(11) 0.0080(9) 0.0129(9) 0.0134(10)
Ge1 0.0116(2) 0.0116(2) 0.0153(3) 0.000 0.000 0.00579(11)

_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
C1 N1 1.493(4) . ?
C2 N1 1.481(7) . ?
N1 C1 1.493(4) 2_665 ?
N1 C1 1.493(4) 3_565 ?
F1 Ge1 1.784(2) . ?
Ge1 F1 1.784(2) 18_655 ?
Ge1 F1 1.784(2) 2_775 ?
Ge1 F1 1.784(2) 16_675 ?
Ge1 F1 1.784(2) 3_575 ?
Ge1 F1 1.784(2) 17_455 ?

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 N1 C1 109.8(2) 2_665 . ?
C1 N1 C1 109.8(2) . 3_565 ?
C1 N1 C1 109.8(2) 2_665 3_565 ?
C2 N1 C1 109.2(2) . 3_565 ?
C2 N1 C1 109.2(2) . 2_665 ?
C2 N1 C1 109.2(2) . . ?
F1 Ge1 F1 90.37(13) 18_655 16_675 ?
F1 Ge1 F1 89.63(13) 16_675 2_775 ?
F1 Ge1 F1 89.63(13) 18_655 2_775 ?
F1 Ge1 F1 180.0 2_775 17_455 ?
F1 Ge1 F1 89.63(13) 17_455 3_575 ?
F1 Ge1 F1 90.37(13) 18_655 17_455 ?
F1 Ge1 F1 90.37(13) 2_775 3_575 ?
F1 Ge1 F1 180.0 16_675 . ?
F1 Ge1 F1 90.37(13) 2_775 . ?
F1 Ge1 F1 89.63(13) 16_675 3_575 ?
F1 Ge1 F1 89.63(13) 18_655 . ?
F1 Ge1 F1 89.63(13) 17_455 . ?
F1 Ge1 F1 180.0 18_655 3_575 ?
F1 Ge1 F1 90.37(13) 16_675 17_455 ?
F1 Ge1 F1 90.37(13) . 3_575 ?

_iucr_refine_instructions_details 
;
    Ge.res created by SHELXL-2014/7

TITL Ge.res in R-3
REM Old TITL Ge in R3
REM SHELXT solution in R-3
REM R1 0.100, Rweak 0.112, Alpha 0.049, Orientation as input
REM Formula found by SHELXT: C10 F6 Ge
CELL 0.71073 7.8554 7.8554 19.6666 90 90 120
ZERR 3.00006 0.0005 0.0005 0.0017 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SFAC C H F Ge N
UNIT 24 72 18 3 6
 
L.S. 5
PLAN  20
SIZE 0.2 0.25 0.3
list 4
fmap 2 53
ACTA
OMIT 1 2 2
OMIT -2 6 1
OMIT -3 3 6
REM <olex2.extras>
REM <HklSrc "%.\\Ge.hkl">
REM </olex2.extras>
 
WGHT    0.075300    9.938999
FVAR       0.58625
C1    1    0.536839    0.802936    0.443779    11.00000    0.01874    0.03238 =
         0.02860   -0.00210   -0.00533    0.00853
AFIX 137
H1B   2    0.622774    0.756062    0.429240    11.00000   -1.50000
H1C   2    0.536409    0.808367    0.492540    11.00000   -1.50000
H1A   2    0.582151    0.931976    0.425573    11.00000   -1.50000
AFIX   0
C2    1    0.333333    0.666667    0.343549    10.33333    0.03554    0.03554 =
         0.01476    0.00000    0.00000    0.01777
PART -1
AFIX 137
H2B   2    0.201635    0.584472    0.327277    10.33333   -1.50000
H2C   2    0.415528    0.617163    0.327277    10.33333   -1.50000
H2A   2    0.382837    0.798365    0.327277    10.33333   -1.50000
AFIX   0
PART 0
N1    5    0.333333    0.666667    0.418862    10.33333    0.01375    0.01375 =
         0.01702    0.00000    0.00000    0.00688
F1    3    0.458886    1.182422    0.385358    11.00000    0.03116    0.03514 =
         0.03250    0.00799    0.01288    0.01336
GE1   4    0.666667    1.333333    0.333333    10.16667    0.01157    0.01157 =
         0.01531    0.00000    0.00000    0.00579
HKLF 4
 
REM  Ge.res in R-3
REM R1 =  0.0668 for    1105 Fo > 4sig(Fo)  and  0.0671 for all    1112 data
REM     29 parameters refined using      0 restraints
 
END  
     
WGHT      0.0752      9.9389 

REM Highest difference peak  2.138,  deepest hole -1.243,  1-sigma level  0.188
Q1    1   0.4599  1.2806  0.3860  11.00000  0.05    2.14
Q2    1   0.6220  1.3618  0.3657  11.00000  0.05    1.96
Q3    1   0.5468  1.2316  0.3421  11.00000  0.05    0.82
Q4    1   0.5360  0.7128  0.4388  11.00000  0.05    0.71
Q5    1   0.3002  0.7006  0.4455  11.00000  0.05    0.56
Q6    1   0.5582  0.9217  0.4451  11.00000  0.05    0.50
Q7    1   0.3708  1.1100  0.3418  11.00000  0.05    0.48
Q8    1   0.3478  1.0713  0.3308  11.00000  0.05    0.48
Q9    1   0.5751  0.7695  0.4142  11.00000  0.05    0.47
Q10   1   0.3333  0.6667  0.5003  10.33333  0.05    0.46
Q11   1   0.5428  1.2054  0.4203  11.00000  0.05    0.46
Q12   1   0.4151  1.3305  0.3570  11.00000  0.05    0.45
Q13   1   0.4684  1.0932  0.4330  11.00000  0.05    0.42
Q14   1   0.3438  0.6028  0.3206  11.00000  0.05    0.40
Q15   1   0.4842  0.8709  0.3880  11.00000  0.05    0.37
Q16   1   0.5278  1.0306  0.4106  11.00000  0.05    0.37
Q17   1   0.5100  1.1330  0.3363  11.00000  0.05    0.35
Q18   1   0.4679  0.8332  0.4824  11.00000  0.05    0.35
Q19   1   0.5467  0.9785  0.3771  11.00000  0.05    0.35
Q20   1   0.7604  0.9215  0.5384  11.00000  0.05    0.34

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0668 for 1105 Fo > 4sig(Fo) and 0.0671 for all 3581 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 2.14, deepest hole -1.24
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0671
  REM R1_gt = 0.0668
  REM wR_ref = 0.1740
  REM GOOF = 1.149
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 3581
  REM Reflections_gt = 1105
  REM Parameters = n/a
  REM Hole = -1.24
  REM Peak = 2.14
  REM Flack = n/a
;
_olex2_date_sample_data_collection 2020-07-10
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.757
_oxdiff_exptl_absorpt_empirical_full_min 0.679
####################################################################### 
# 
# 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_Ge_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2141589'
loop_
_audit_author_name
_audit_author_address
'Jiang Long'
;Sun Yat Sen Universit
China
;
_audit_update_record             
;
2022-01-12 deposited with the CCDC.	2022-02-22 downloaded from the CCDC.
;
_audit_creation_date             2021-12-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'F6 Ge, 2(C4 H12 N)'
_chemical_formula_sum            'C8 H24 F6 Ge N2'
_chemical_formula_weight         334.88
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNFGe
_chemical_oxdiff_usercomment     ?
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'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_H-M_alt        'F m -3 m'
_space_group_name_Hall           '-F 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'z, x+1/2, y+1/2'
'z, -x+1/2, -y+1/2'
'-z, -x+1/2, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z+1/2, x+1/2'
'-y, z+1/2, -x+1/2'
'y, -z+1/2, -x+1/2'
'-y, -z+1/2, x+1/2'
'y, x+1/2, -z+1/2'
'-y, -x+1/2, -z+1/2'
'y, -x+1/2, z+1/2'
'-y, x+1/2, z+1/2'
'x, z+1/2, -y+1/2'
'-x, z+1/2, y+1/2'
'-x, -z+1/2, -y+1/2'
'x, -z+1/2, y+1/2'
'z, y+1/2, -x+1/2'
'z, -y+1/2, x+1/2'
'-z, y+1/2, x+1/2'
'-z, -y+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+1/2, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'z+1/2, x, y+1/2'
'z+1/2, -x, -y+1/2'
'-z+1/2, -x, y+1/2'
'-z+1/2, x, -y+1/2'
'y+1/2, z, x+1/2'
'-y+1/2, z, -x+1/2'
'y+1/2, -z, -x+1/2'
'-y+1/2, -z, x+1/2'
'y+1/2, x, -z+1/2'
'-y+1/2, -x, -z+1/2'
'y+1/2, -x, z+1/2'
'-y+1/2, x, z+1/2'
'x+1/2, z, -y+1/2'
'-x+1/2, z, y+1/2'
'-x+1/2, -z, -y+1/2'
'x+1/2, -z, y+1/2'
'z+1/2, y, -x+1/2'
'z+1/2, -y, x+1/2'
'-z+1/2, y, x+1/2'
'-z+1/2, -y, -x+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'z+1/2, x+1/2, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x+1/2, y'
'-z+1/2, x+1/2, -y'
'y+1/2, z+1/2, x'
'-y+1/2, z+1/2, -x'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z+1/2, x'
'y+1/2, x+1/2, -z'
'-y+1/2, -x+1/2, -z'
'y+1/2, -x+1/2, z'
'-y+1/2, x+1/2, z'
'x+1/2, z+1/2, -y'
'-x+1/2, z+1/2, y'
'-x+1/2, -z+1/2, -y'
'x+1/2, -z+1/2, y'
'z+1/2, y+1/2, -x'
'z+1/2, -y+1/2, x'
'-z+1/2, y+1/2, x'
'-z+1/2, -y+1/2, -x'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'
'-x, -y+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
'-x, y+1/2, z+1/2'
'-z, -x+1/2, -y+1/2'
'-z, x+1/2, y+1/2'
'z, x+1/2, -y+1/2'
'z, -x+1/2, y+1/2'
'-y, -z+1/2, -x+1/2'
'y, -z+1/2, x+1/2'
'-y, z+1/2, x+1/2'
'y, z+1/2, -x+1/2'
'-y, -x+1/2, z+1/2'
'y, x+1/2, z+1/2'
'-y, x+1/2, -z+1/2'
'y, -x+1/2, -z+1/2'
'-x, -z+1/2, y+1/2'
'x, -z+1/2, -y+1/2'
'x, z+1/2, y+1/2'
'-x, z+1/2, -y+1/2'
'-z, -y+1/2, x+1/2'
'-z, y+1/2, -x+1/2'
'z, -y+1/2, -x+1/2'
'z, y+1/2, x+1/2'
'-x+1/2, -y, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y, z+1/2'
'-z+1/2, -x, -y+1/2'
'-z+1/2, x, y+1/2'
'z+1/2, x, -y+1/2'
'z+1/2, -x, y+1/2'
'-y+1/2, -z, -x+1/2'
'y+1/2, -z, x+1/2'
'-y+1/2, z, x+1/2'
'y+1/2, z, -x+1/2'
'-y+1/2, -x, z+1/2'
'y+1/2, x, z+1/2'
'-y+1/2, x, -z+1/2'
'y+1/2, -x, -z+1/2'
'-x+1/2, -z, y+1/2'
'x+1/2, -z, -y+1/2'
'x+1/2, z, y+1/2'
'-x+1/2, z, -y+1/2'
'-z+1/2, -y, x+1/2'
'-z+1/2, y, -x+1/2'
'z+1/2, -y, -x+1/2'
'z+1/2, y, x+1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-z+1/2, -x+1/2, -y'
'-z+1/2, x+1/2, y'
'z+1/2, x+1/2, -y'
'z+1/2, -x+1/2, y'
'-y+1/2, -z+1/2, -x'
'y+1/2, -z+1/2, x'
'-y+1/2, z+1/2, x'
'y+1/2, z+1/2, -x'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'
'-y+1/2, x+1/2, -z'
'y+1/2, -x+1/2, -z'
'-x+1/2, -z+1/2, y'
'x+1/2, -z+1/2, -y'
'x+1/2, z+1/2, y'
'-x+1/2, z+1/2, -y'
'-z+1/2, -y+1/2, x'
'-z+1/2, y+1/2, -x'
'z+1/2, -y+1/2, -x'
'z+1/2, y+1/2, x'

_cell_length_a                   11.2682(18)
_cell_length_b                   11.2682(18)
_cell_length_c                   11.2682(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1430.8(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    359
_cell_measurement_temperature    292.99(10)
_cell_measurement_theta_max      29.7250
_cell_measurement_theta_min      3.5890
_shelx_estimated_absorpt_T_max   0.917
_shelx_estimated_absorpt_T_min   0.880
_exptl_absorpt_coefficient_mu    2.191
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50531
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1790
_diffrn_reflns_av_unetI/netI     0.0889
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            610
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.978
_diffrn_reflns_theta_min         3.131
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -42.00   0.00   1.00   20.00    --  -12.93 -77.00  30.00   42
  2  ω   -105.00 -76.00   1.00   20.00    --  -18.01 178.00-180.00   29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0267451000
_diffrn_orient_matrix_UB_12      0.0391881000
_diffrn_orient_matrix_UB_13      0.0416499000
_diffrn_orient_matrix_UB_21      -0.0398202000
_diffrn_orient_matrix_UB_22      -0.0457251000
_diffrn_orient_matrix_UB_23      0.0173705000
_diffrn_orient_matrix_UB_31      0.0406919000
_diffrn_orient_matrix_UB_32      -0.0184450000
_diffrn_orient_matrix_UB_33      0.0439031000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                122
_reflns_number_total             127
_reflns_odcompleteness_completeness 99.14
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.063
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.182
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     9
_refine_ls_number_reflns         127
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0862
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1555P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2249
_refine_ls_wR_factor_ref         0.2289
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H) groups
2.a Riding coordinates:
 C1(H1)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Ge1 Ge 0.5000 0.5000 0.5000 0.0293(12) Uani 1 48 d S T P . .
N1 N 0.7500 0.7500 0.7500 0.036(4) Uani 1 24 d S T P . .
F1 F 0.5000 0.5000 0.6559(10) 0.119(7) Uani 1 8 d S T P . .
C1 C 0.6732(8) 0.6732(8) 0.8268(8) 0.073(5) Uani 1 6 d S T P . .
H1 H 0.6246 0.6246 0.7776 0.110 Uiso 1 2 d RS T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ge1 0.0293(12) 0.0293(12) 0.0293(12) 0.000 0.000 0.000
N1 0.036(4) 0.036(4) 0.036(4) 0.000 0.000 0.000
F1 0.172(11) 0.172(11) 0.013(4) 0.000 0.000 0.000
C1 0.073(5) 0.073(5) 0.073(5) 0.019(4) 0.019(4) -0.019(4)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 F1 1.757(11) . ?
Ge1 F1 1.757(11) 5 ?
Ge1 F1 1.757(11) 101_666 ?
Ge1 F1 1.757(11) 97_666 ?
Ge1 F1 1.757(11) 105_666 ?
Ge1 F1 1.757(11) 9 ?
N1 C1 1.498(15) 74_665 ?
N1 C1 1.498(15) 28_566 ?
N1 C1 1.498(15) 51_656 ?
N1 C1 1.498(15) . ?
C1 H1 0.9519 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F1 Ge1 F1 90.0 . 105_666 ?
F1 Ge1 F1 90.000(1) 105_666 5 ?
F1 Ge1 F1 90.000(3) 105_666 101_666 ?
F1 Ge1 F1 180.0 5 101_666 ?
F1 Ge1 F1 90.000(1) 105_666 97_666 ?
F1 Ge1 F1 90.0 . 101_666 ?
F1 Ge1 F1 180.0 . 97_666 ?
F1 Ge1 F1 90.000(2) 97_666 101_666 ?
F1 Ge1 F1 180.0 105_666 9 ?
F1 Ge1 F1 90.0 97_666 5 ?
F1 Ge1 F1 90.000(1) . 9 ?
F1 Ge1 F1 90.000(2) 5 9 ?
F1 Ge1 F1 90.0 97_666 9 ?
F1 Ge1 F1 90.000(2) . 5 ?
F1 Ge1 F1 90.000(1) 101_666 9 ?
C1 N1 C1 109.471(2) 74_665 28_566 ?
C1 N1 C1 109.471(5) 74_665 51_656 ?
C1 N1 C1 109.471(3) 28_566 . ?
C1 N1 C1 109.471(1) 74_665 . ?
C1 N1 C1 109.471(1) 28_566 51_656 ?
C1 N1 C1 109.471(2) 51_656 . ?
N1 C1 H1 109.2 . . ?

_iucr_refine_instructions_details 
;

    Ge.res created by SHELXL-2014/7

TITL Ge.res in Fm-3m
REM Old TITL Ge in F-43m
REM SHELXT solution in Fm-3m
REM R1 0.227, Rweak 0.168, Alpha 0.050, Orientation as input
REM Formula found by SHELXT: C2 F14 Ge
CELL 0.71073 11.268203 11.268203 11.268203 90 90 90
ZERR 4 0.001757 0.001757 0.001757 0 0 0
LATT 4
SYMM -X,-Y,+Z
SYMM -X,+Y,-Z
SYMM +X,-Y,-Z
SYMM +Z,+X,+Y
SYMM +Z,-X,-Y
SYMM -Z,-X,+Y
SYMM -Z,+X,-Y
SYMM +Y,+Z,+X
SYMM -Y,+Z,-X
SYMM +Y,-Z,-X
SYMM -Y,-Z,+X
SYMM +Y,+X,-Z
SYMM -Y,-X,-Z
SYMM +Y,-X,+Z
SYMM -Y,+X,+Z
SYMM +X,+Z,-Y
SYMM -X,+Z,+Y
SYMM -X,-Z,-Y
SYMM +X,-Z,+Y
SYMM +Z,+Y,-X
SYMM +Z,-Y,+X
SYMM -Z,+Y,+X
SYMM -Z,-Y,-X
SFAC C H F Ge N
UNIT 32 96 24 4 8
 
L.S. 4
PLAN  20
SIZE 0.04 0.05 0.06
BOND $H
list 4
fmap 2
acta
OMIT -3 58
OMIT 4 6 8
OMIT 2 4 4
OMIT 1 3 3
REM <olex2.extras>
REM <HklSrc "%.\\Ge.hkl">
REM </olex2.extras>
 
WGHT    0.155500
FVAR       2.67205
GE1   4    0.500000    0.500000    0.500000    10.02083    0.02934    0.02934 =
         0.02934    0.00000    0.00000    0.00000
N1    5    0.750000    0.750000    0.750000    10.04167    0.03642    0.03642 =
         0.03642    0.00000    0.00000    0.00000
F1    3    0.500000    0.500000    0.655917    10.12500    0.17175    0.17175 =
         0.01334    0.00000    0.00000    0.00000
C1    1    0.673235    0.673235    0.826765    10.16667    0.07312    0.07312 =
         0.07312    0.01911    0.01911   -0.01911
AFIX   3
H1    2    0.624635    0.624640    0.777640    10.50000   -1.50000
AFIX   0
HKLF 4
 
REM  Ge.res in Fm-3m
REM R1 =  0.0862 for     122 Fo > 4sig(Fo)  and  0.0880 for all     127 data
REM      9 parameters refined using      0 restraints
 
END  
     
WGHT      0.1555      0.0000 

REM Highest difference peak  1.063,  deepest hole -0.673,  1-sigma level  0.182
Q1    1   0.4548  0.5000  0.5000  10.12500  0.05    1.06
Q2    1   0.5000  0.5000  0.7040  10.12500  0.05    1.02
Q3    1   0.5000  0.5000  0.5740  10.12500  0.05    1.00
Q4    1   0.7500  0.6051  0.7500  10.25000  0.05    0.49
Q5    1   0.6952  0.5982  0.6952  10.50000  0.05    0.38
Q6    1   0.5449  0.5000  0.6377  10.50000  0.05    0.37
Q7    1   0.5573  0.6701  0.6701  10.50000  0.05    0.32
Q8    1   0.5879  0.6694  0.8306  10.50000  0.05    0.31
Q9    1   0.5686  0.5686  0.7701  10.50000  0.05    0.28
Q10   1   0.5000  0.5528  0.9472  10.25000  0.05    0.28
Q11   1   0.5000  0.5000  0.8620  10.12500  0.05    0.28
Q12   1   0.5000  0.6303  0.7152  10.50000  0.05    0.23
Q13   1   0.5000  0.6733  0.8267  10.25000  0.05    0.22
Q14   1   0.5898  0.5898  0.7005  10.50000  0.05    0.20
Q15   1   0.5752  0.5752  0.8406  10.50000  0.05    0.20
Q16   1   0.5000  0.6765  0.7003  10.50000  0.05    0.18
Q17   1   0.5523  0.5000  0.8956  10.50000  0.05    0.15
Q18   1   0.7022  0.7978  0.7978  10.16667  0.05    0.13
Q19   1   0.6061  0.5000  0.7341  10.50000  0.05    0.08
Q20   1   0.6393  0.5000  0.7947  10.50000  0.05    0.08

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0862 for 122 Fo > 4sig(Fo) and 0.0880 for all 665 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 1.06, deepest hole -0.67
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0880
  REM R1_gt = 0.0862
  REM wR_ref = 0.2289
  REM GOOF = 1.101
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 665
  REM Reflections_gt = 122
  REM Parameters = n/a
  REM Hole = -0.67
  REM Peak = 1.06
  REM Flack = n/a

  
;
_olex2_date_sample_data_collection 2021-12-09
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.882
_oxdiff_exptl_absorpt_empirical_full_min 0.375
####################################################################### 
# 
# 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_Ti_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2141585'
loop_
_audit_author_name
_audit_author_address
'Jiang Long'
;Sun Yat Sen Universit
China
;
_audit_update_record             
;
2022-01-12 deposited with the CCDC.	2022-02-22 downloaded from the CCDC.
;
_audit_creation_date             2021-12-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'F6 Ti, 2(C4 H12 N)'
_chemical_formula_sum            'C8 H24 F6 N2 Ti'
_chemical_formula_weight         310.24
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNFTi
_chemical_oxdiff_usercomment     ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_H-M_alt        'F m -3 m'
_space_group_name_Hall           '-F 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'z, x+1/2, y+1/2'
'z, -x+1/2, -y+1/2'
'-z, -x+1/2, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z+1/2, x+1/2'
'-y, z+1/2, -x+1/2'
'y, -z+1/2, -x+1/2'
'-y, -z+1/2, x+1/2'
'y, x+1/2, -z+1/2'
'-y, -x+1/2, -z+1/2'
'y, -x+1/2, z+1/2'
'-y, x+1/2, z+1/2'
'x, z+1/2, -y+1/2'
'-x, z+1/2, y+1/2'
'-x, -z+1/2, -y+1/2'
'x, -z+1/2, y+1/2'
'z, y+1/2, -x+1/2'
'z, -y+1/2, x+1/2'
'-z, y+1/2, x+1/2'
'-z, -y+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+1/2, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'z+1/2, x, y+1/2'
'z+1/2, -x, -y+1/2'
'-z+1/2, -x, y+1/2'
'-z+1/2, x, -y+1/2'
'y+1/2, z, x+1/2'
'-y+1/2, z, -x+1/2'
'y+1/2, -z, -x+1/2'
'-y+1/2, -z, x+1/2'
'y+1/2, x, -z+1/2'
'-y+1/2, -x, -z+1/2'
'y+1/2, -x, z+1/2'
'-y+1/2, x, z+1/2'
'x+1/2, z, -y+1/2'
'-x+1/2, z, y+1/2'
'-x+1/2, -z, -y+1/2'
'x+1/2, -z, y+1/2'
'z+1/2, y, -x+1/2'
'z+1/2, -y, x+1/2'
'-z+1/2, y, x+1/2'
'-z+1/2, -y, -x+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'z+1/2, x+1/2, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x+1/2, y'
'-z+1/2, x+1/2, -y'
'y+1/2, z+1/2, x'
'-y+1/2, z+1/2, -x'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z+1/2, x'
'y+1/2, x+1/2, -z'
'-y+1/2, -x+1/2, -z'
'y+1/2, -x+1/2, z'
'-y+1/2, x+1/2, z'
'x+1/2, z+1/2, -y'
'-x+1/2, z+1/2, y'
'-x+1/2, -z+1/2, -y'
'x+1/2, -z+1/2, y'
'z+1/2, y+1/2, -x'
'z+1/2, -y+1/2, x'
'-z+1/2, y+1/2, x'
'-z+1/2, -y+1/2, -x'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'
'-x, -y+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
'-x, y+1/2, z+1/2'
'-z, -x+1/2, -y+1/2'
'-z, x+1/2, y+1/2'
'z, x+1/2, -y+1/2'
'z, -x+1/2, y+1/2'
'-y, -z+1/2, -x+1/2'
'y, -z+1/2, x+1/2'
'-y, z+1/2, x+1/2'
'y, z+1/2, -x+1/2'
'-y, -x+1/2, z+1/2'
'y, x+1/2, z+1/2'
'-y, x+1/2, -z+1/2'
'y, -x+1/2, -z+1/2'
'-x, -z+1/2, y+1/2'
'x, -z+1/2, -y+1/2'
'x, z+1/2, y+1/2'
'-x, z+1/2, -y+1/2'
'-z, -y+1/2, x+1/2'
'-z, y+1/2, -x+1/2'
'z, -y+1/2, -x+1/2'
'z, y+1/2, x+1/2'
'-x+1/2, -y, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y, z+1/2'
'-z+1/2, -x, -y+1/2'
'-z+1/2, x, y+1/2'
'z+1/2, x, -y+1/2'
'z+1/2, -x, y+1/2'
'-y+1/2, -z, -x+1/2'
'y+1/2, -z, x+1/2'
'-y+1/2, z, x+1/2'
'y+1/2, z, -x+1/2'
'-y+1/2, -x, z+1/2'
'y+1/2, x, z+1/2'
'-y+1/2, x, -z+1/2'
'y+1/2, -x, -z+1/2'
'-x+1/2, -z, y+1/2'
'x+1/2, -z, -y+1/2'
'x+1/2, z, y+1/2'
'-x+1/2, z, -y+1/2'
'-z+1/2, -y, x+1/2'
'-z+1/2, y, -x+1/2'
'z+1/2, -y, -x+1/2'
'z+1/2, y, x+1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-z+1/2, -x+1/2, -y'
'-z+1/2, x+1/2, y'
'z+1/2, x+1/2, -y'
'z+1/2, -x+1/2, y'
'-y+1/2, -z+1/2, -x'
'y+1/2, -z+1/2, x'
'-y+1/2, z+1/2, x'
'y+1/2, z+1/2, -x'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'
'-y+1/2, x+1/2, -z'
'y+1/2, -x+1/2, -z'
'-x+1/2, -z+1/2, y'
'x+1/2, -z+1/2, -y'
'x+1/2, z+1/2, y'
'-x+1/2, z+1/2, -y'
'-z+1/2, -y+1/2, x'
'-z+1/2, y+1/2, -x'
'z+1/2, -y+1/2, -x'
'z+1/2, y+1/2, x'

_cell_length_a                   11.372(3)
_cell_length_b                   11.372(3)
_cell_length_c                   11.372(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1470.8(13)
_cell_formula_units_Z            3.99936
_cell_measurement_reflns_used    141
_cell_measurement_temperature    293.00(10)
_cell_measurement_theta_max      22.6300
_cell_measurement_theta_min      5.0460
_shelx_estimated_absorpt_T_max   0.981
_shelx_estimated_absorpt_T_min   0.963
_exptl_absorpt_coefficient_mu    0.630
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1075
_diffrn_reflns_av_unetI/netI     0.0677
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.879
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            399
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.256
_diffrn_reflns_theta_min         3.103
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -8.00  32.00   1.00   30.00    --   14.02 -57.00  30.00   40
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0065204000
_diffrn_orient_matrix_UB_12      -0.0569469000
_diffrn_orient_matrix_UB_13      -0.0247288000
_diffrn_orient_matrix_UB_21      0.0495680000
_diffrn_orient_matrix_UB_22      0.0200205000
_diffrn_orient_matrix_UB_23      -0.0324753000
_diffrn_orient_matrix_UB_31      0.0373554000
_diffrn_orient_matrix_UB_32      -0.0157146000
_diffrn_orient_matrix_UB_33      0.0471146000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                99
_reflns_number_total             131
_reflns_odcompleteness_completeness 98.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.137
_refine_ls_extinction_coef       0.07(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     10
_refine_ls_number_reflns         131
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1110
_refine_ls_R_factor_gt           0.1017
_refine_ls_restrained_S_all      0.972
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2533
_refine_ls_wR_factor_ref         0.2688
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H1B(0.16667) H1C(0.16667) H1A(0.16667)
3.a Riding coordinates:
 C1(H1B,H1C,H1A)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Ti1 Ti 0.5000 0.5000 0.5000 0.0459(18) Uani 1 48 d S T P . .
N1 N 0.7500 0.7500 0.7500 0.050(3) Uani 1 24 d S T P . .
F1 F 0.6602(7) 0.5000 0.5000 0.111(4) Uani 1 8 d S T P . .
C1 C 0.8256(4) 0.6744(4) 0.6744(4) 0.085(4) Uani 1 6 d S T P . .
H1B H 0.8689 0.6310 0.7235 0.127 Uiso 0.3333 2 d RS T P . .
H1C H 0.8795 0.7235 0.6204 0.127 Uiso 0.3333 2 d RS T P . .
H1A H 0.7772 0.6318 0.6318 0.127 Uiso 0.3333 2 d RS T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ti1 0.0459(18) 0.0459(18) 0.0459(18) 0.000 0.000 0.000
N1 0.050(3) 0.050(3) 0.050(3) 0.000 0.000 0.000
F1 0.043(4) 0.146(6) 0.146(6) 0.000 0.000 0.000
C1 0.085(4) 0.085(4) 0.085(4) -0.021(3) 0.021(3) 0.021(3)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 F1 1.822(8) . ?
Ti1 F1 1.822(8) 9 ?
Ti1 F1 1.822(8) 5 ?
Ti1 F1 1.822(8) 105_666 ?
Ti1 F1 1.822(8) 97_666 ?
Ti1 F1 1.822(8) 101_666 ?
N1 C1 1.490(9) 51_656 ?
N1 C1 1.490(9) . ?
N1 C1 1.490(9) 74_665 ?
N1 C1 1.490(9) 28_566 ?
C1 H1B 0.8927 . ?
C1 H1C 1.0318 . ?
C1 H1A 0.8793 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F1 Ti1 F1 90.000(1) . 105_666 ?
F1 Ti1 F1 90.000(2) 97_666 101_666 ?
F1 Ti1 F1 90.000(1) 97_666 9 ?
F1 Ti1 F1 180.0 . 97_666 ?
F1 Ti1 F1 90.000(1) . 9 ?
F1 Ti1 F1 90.000(2) 105_666 97_666 ?
F1 Ti1 F1 90.000(1) 105_666 101_666 ?
F1 Ti1 F1 90.000(2) . 5 ?
F1 Ti1 F1 180.0 5 101_666 ?
F1 Ti1 F1 90.0 105_666 5 ?
F1 Ti1 F1 180.0 105_666 9 ?
F1 Ti1 F1 90.000(1) 97_666 5 ?
F1 Ti1 F1 90.000(1) 101_666 9 ?
F1 Ti1 F1 90.000(1) . 101_666 ?
F1 Ti1 F1 90.000(1) 5 9 ?
C1 N1 C1 109.5 28_566 51_656 ?
C1 N1 C1 109.5 51_656 . ?
C1 N1 C1 109.471(3) 28_566 . ?
C1 N1 C1 109.471(2) 28_566 74_665 ?
C1 N1 C1 109.471(2) 51_656 74_665 ?
C1 N1 C1 109.5 74_665 . ?
N1 C1 H1B 106.0 . . ?
N1 C1 H1C 112.0 . . ?
N1 C1 H1A 105.9 . . ?
H1B C1 H1C 110.1 . . ?
H1B C1 H1A 112.7 . . ?
H1C C1 H1A 110.0 . . ?

_iucr_refine_instructions_details 
;

    Ti.res created by SHELXL-2014/7

TITL Ti.res in Fm-3m
REM Old TITL Ti.res in F-43m
REM SHELXT solution in Fm-3m
REM R1 0.220, Rweak 0.213, Alpha 0.092, Orientation as input
REM Formula found by SHELXT: C2 F14 Ti
CELL 0.71073 11.3724 11.3724 11.3724 90 90 90
ZERR 3.99936 0.0033 0.0033 0.0033 0 0 0
LATT 4
SYMM -X,-Y,+Z
SYMM -X,+Y,-Z
SYMM +X,-Y,-Z
SYMM +Z,+X,+Y
SYMM +Z,-X,-Y
SYMM -Z,-X,+Y
SYMM -Z,+X,-Y
SYMM +Y,+Z,+X
SYMM -Y,+Z,-X
SYMM +Y,-Z,-X
SYMM -Y,-Z,+X
SYMM +Y,+X,-Z
SYMM -Y,-X,-Z
SYMM +Y,-X,+Z
SYMM -Y,+X,+Z
SYMM +X,+Z,-Y
SYMM -X,+Z,+Y
SYMM -X,-Z,-Y
SYMM +X,-Z,+Y
SYMM +Z,+Y,-X
SYMM +Z,-Y,+X
SYMM -Z,+Y,+X
SYMM -Z,-Y,-X
SFAC C H F N Ti
UNIT 32 96 24 8 4
 
L.S. 50
PLAN  20
SIZE 0.03 0.04 0.06
BOND $H
list 4
fmap 2
acta
OMIT 3 5 9
OMIT 2 4 8
OMIT 1 3 9
REM <olex2.extras>
REM <HklSrc "%.\\exp_2585.hkl">
REM </olex2.extras>
 
WGHT    0.200000
EXTI    0.072140
FVAR       2.28801
TI1   5    0.500000    0.500000    0.500000    10.02083    0.04593    0.04593 =
         0.04593    0.00000    0.00000    0.00000
N1    4    0.750000    0.750000    0.750000    10.04167    0.05011    0.05011 =
         0.05011    0.00000    0.00000    0.00000
F1    3    0.660232    0.500000    0.500000    10.12500    0.04288    0.14551 =
         0.14551    0.00000    0.00000    0.00000
C1    1    0.825625    0.674375    0.674375    10.16667    0.08482    0.08482 =
         0.08482   -0.02088    0.02088    0.02088
AFIX   3
H1B   2    0.868885    0.631010    0.723470    10.16667   -1.50000
H1C   2    0.879525    0.723470    0.620370    10.16667   -1.50000
H1A   2    0.777185    0.631760    0.631760    10.16667   -1.50000
AFIX   0
HKLF 4
 
REM  Ti.res in Fm-3m
REM R1 =  0.1017 for      99 Fo > 4sig(Fo)  and  0.1110 for all     131 data
REM     10 parameters refined using      0 restraints
 
END  
     
WGHT      0.1476      0.0000 

REM Highest difference peak  0.696,  deepest hole -0.683,  1-sigma level  0.137
Q1    1   1.0000  0.5000  0.5000  10.02083  0.05    0.70
Q2    1   0.5806  0.5000  0.5807  10.25000  0.05    0.69
Q3    1   0.8344  0.6656  0.8344  10.16667  0.05    0.39
Q4    1   0.8113  0.6887  0.6887  10.16667  0.05    0.27
Q5    1   0.8525  0.8094  0.5000  10.50000  0.05    0.26
Q6    1   0.6566  0.4265  0.5735  10.50000  0.05    0.19
Q7    1   0.8729  0.8065  0.5421  11.00000  0.05    0.16
Q8    1   0.8877  0.8200  0.5647  11.00000  0.05    0.16
Q9    1   0.9158  0.8285  0.5842  10.50000  0.05    0.16
Q10   1   0.8184  0.7500  0.7500  10.25000  0.05    0.11
Q11   1   0.7294  0.5000  0.5720  10.50000  0.05    0.11
Q12   1   0.6949  0.5000  0.5000  10.12500  0.05    0.10
Q13   1   0.6965  0.5323  0.5000  10.50000  0.05    0.10
Q14   1   0.7616  0.7616  0.5000  10.25000  0.05    0.07

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.1017 for 99 Fo > 4sig(Fo) and 0.1110 for all 417 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.70, deepest hole -0.68
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.1110
  REM R1_gt = 0.1017
  REM wR_ref = 0.2688
  REM GOOF = 0.972
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 417
  REM Reflections_gt = 99
  REM Parameters = n/a
  REM Hole = -0.68
  REM Peak = 0.70
  REM Flack = n/a

  
;
_olex2_date_sample_data_collection 2021-12-09
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.958
_oxdiff_exptl_absorpt_empirical_full_min 0.403
####################################################################### 
# 
# 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_Si_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2141587'
loop_
_audit_author_name
_audit_author_address
'Jiang Long'
;Sun Yat Sen Universit
China
;
_audit_update_record             
;
2022-01-12 deposited with the CCDC.	2022-02-22 downloaded from the CCDC.
;
_audit_creation_date             2021-12-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'F6 Si, 2(C4 H12 N)'
_chemical_formula_sum            'C8 H24 F6 N2 Si'
_chemical_formula_weight         290.38
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_H-M_alt        'I 4/m'
_space_group_name_Hall           '-I 4'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'

_cell_length_a                   7.8924(10)
_cell_length_b                   7.8924(10)
_cell_length_c                   11.163(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     695.3(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    293.00(10)
_cell_measurement_theta_max      30.0460
_cell_measurement_theta_min      3.6000
_shelx_estimated_absorpt_T_max   0.968
_shelx_estimated_absorpt_T_min   0.937
_exptl_absorpt_coefficient_mu    0.220
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.08748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             308
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0692
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            493
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.292
_diffrn_reflns_theta_min         3.161
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -53.00 -21.00   1.00    3.00    --  -13.08  19.00 120.00   32
  2  ω     -8.00  65.00   1.00    3.00    --  -13.08  19.00 120.00   73
  3  ω    -73.00   7.00   1.00    3.00    --  -13.08 -38.00   0.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0885190000
_diffrn_orient_matrix_UB_12      0.0738142000
_diffrn_orient_matrix_UB_13      -0.0130815000
_diffrn_orient_matrix_UB_21      -0.0539704000
_diffrn_orient_matrix_UB_22      0.0543896000
_diffrn_orient_matrix_UB_23      -0.0266333000
_diffrn_orient_matrix_UB_31      0.0734870000
_diffrn_orient_matrix_UB_32      0.0608833000
_diffrn_orient_matrix_UB_33      0.1059364000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                460
_reflns_number_total             493
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     27
_refine_ls_number_reflns         493
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0543
_refine_ls_restrained_S_all      1.143
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0323P)²+0.3439P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1185
_refine_special_details          
;
 Refined as a 4-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.755(10)
 0.122(6) -0.002(3) 0.125(7)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3.a Idealised Me refined as rotating group:
 C1(H1C,H1B,H1A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Si1 Si 0.0000 0.0000 0.5000 0.0237(3) Uani 1 8 d S T P . .
F1 F 0.1807(3) 0.1118(3) 0.5000 0.0527(7) Uani 1 2 d S T P . .
F2 F 0.0000 0.0000 0.3498(4) 0.0651(11) Uani 1 4 d S T P . .
N1 N 0.0000 0.5000 0.2500 0.0276(6) Uani 1 4 d S T P . .
C1 C 0.1518(3) 0.4732(4) 0.3272(2) 0.0441(6) Uani 1 1 d . . . . .
H1C H 0.1373 0.3717 0.3734 0.066 Uiso 1 1 calc GR . . . .
H1B H 0.1650 0.5681 0.3802 0.066 Uiso 1 1 calc GR . . . .
H1A H 0.2507 0.4626 0.2777 0.066 Uiso 1 1 calc GR . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Si1 0.0233(5) 0.0233(5) 0.0246(9) 0.000 0.000 0.000
F1 0.0346(10) 0.0486(12) 0.0750(18) 0.000 0.000 -0.0152(8)
F2 0.0838(17) 0.0838(17) 0.0277(18) 0.000 0.000 0.000
N1 0.0275(10) 0.0275(10) 0.028(2) 0.000 0.000 0.000
C1 0.0356(11) 0.0514(14) 0.0452(16) 0.0014(11) -0.0121(10) 0.0003(9)

_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
Si1 F1 1.677(2) 9_556 ?
Si1 F1 1.677(2) 10_556 ?
Si1 F1 1.677(2) 2 ?
Si1 F1 1.677(2) . ?
Si1 F2 1.676(4) . ?
Si1 F2 1.676(4) 9_556 ?
N1 C1 1.4907(18) . ?
N1 C1 1.4907(18) 3_565 ?
N1 C1 1.4907(18) 14_455 ?
N1 C1 1.4907(18) 16 ?
C1 H1C 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1A 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
F1 Si1 F1 90.0 9_556 10_556 ?
F1 Si1 F1 90.0 10_556 . ?
F1 Si1 F1 90.0 2 . ?
F1 Si1 F1 180.0 9_556 . ?
F1 Si1 F1 90.0 9_556 2 ?
F1 Si1 F1 180.0 10_556 2 ?
F2 Si1 F1 90.0 9_556 2 ?
F2 Si1 F1 90.000(1) 9_556 9_556 ?
F2 Si1 F1 90.0 . . ?
F2 Si1 F1 90.0 9_556 10_556 ?
F2 Si1 F1 90.0 . 10_556 ?
F2 Si1 F1 90.0 . 2 ?
F2 Si1 F1 90.0 9_556 . ?
F2 Si1 F1 90.0 . 9_556 ?
F2 Si1 F2 180.0 9_556 . ?
C1 N1 C1 109.53(12) . 16 ?
C1 N1 C1 109.4(2) . 3_565 ?
C1 N1 C1 109.53(12) 16 3_565 ?
C1 N1 C1 109.4(2) 14_455 16 ?
C1 N1 C1 109.53(12) . 14_455 ?
C1 N1 C1 109.53(12) 14_455 3_565 ?
N1 C1 H1C 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1A 109.5 . . ?
H1C C1 H1B 109.5 . . ?
H1C C1 H1A 109.5 . . ?
H1B C1 H1A 109.5 . . ?

_iucr_refine_instructions_details 
;

    Si.res created by SHELXL-2014/7

TITL Si P -1 R = 0.12 New: I4/m
CELL 0.71073 7.8924 7.8924 11.163 90 90 90
ZERR 2 0.001 0.001 0.004 0 0 0
LATT 2
SYMM -Y,+X,+Z
SYMM -X,-Y,+Z
SYMM +Y,-X,+Z
SFAC C H F N Si
UNIT 16 48 12 4 2
 
L.S. 13
PLAN  -20
SIZE 0.15 0.25 0.3
TEMP 19.85(10)
BOND $H
CONF
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\Si.hkl">
REM </olex2.extras>
 
WGHT    0.032300    0.343900
BASF   0.12176  -0.00175   0.12470
FVAR      31.08810
SI1   5    0.000000    0.000000    0.500000    10.12500    0.02328    0.02328 =
         0.02464    0.00000    0.00000    0.00000
F1    3    0.180710    0.111838    0.500000    10.50000    0.03465    0.04858 =
         0.07500    0.00000    0.00000   -0.01519
F2    3    0.000000    0.000000    0.349845    10.25000    0.08380    0.08380 =
         0.02765    0.00000    0.00000    0.00000
N1    4    0.000000    0.500000    0.250000    10.25000    0.02751    0.02751 =
         0.02782    0.00000    0.00000    0.00000
C1    1    0.151757    0.473212    0.327212    11.00000    0.03555    0.05141 =
         0.04523    0.00139   -0.01208    0.00025
AFIX 137
H1C   2    0.137264    0.371652    0.373416    11.00000   -1.50000
H1B   2    0.165042    0.568097    0.380194    11.00000   -1.50000
H1A   2    0.250697    0.462636    0.277749    11.00000   -1.50000
AFIX   0
HKLF 5
 
REM  Si P -1 R = 0.12 New: I4/m
REM R1 =  0.0543 for     460 Fo > 4sig(Fo)  and  0.0583 for all     493 data
REM     27 parameters refined using      0 restraints
 
END  
     
WGHT      0.0324      0.3464 

REM Highest difference peak  0.258,  deepest hole -0.234,  1-sigma level  0.060
Q1    1   0.0967  0.0240  0.3845  11.00000  0.05    0.26
Q2    1   0.0221  0.1247  0.5000  10.50000  0.05    0.25
Q3    1   0.0000  0.0000  0.0000  10.12500  0.05    0.22
Q4    1   0.0000  0.0000  0.2165  10.25000  0.05    0.21
Q5    1   0.0948  0.1232  0.3236  11.00000  0.05    0.19
Q6    1   0.2470  0.1527  0.3703  11.00000  0.05    0.18
Q7    1   0.1404  0.1220  0.4519  11.00000  0.05    0.18
Q8    1   0.5000  0.0000  0.3073  10.50000  0.05    0.18
Q9    1   0.2441  0.5598  0.5000  10.50000  0.05    0.18
Q10   1  -0.1048  0.0731  0.5000  10.50000  0.05    0.17
Q11   1   0.5127  0.0493  0.3053  11.00000  0.05    0.17
Q12   1   0.3733 -0.0075  0.3661  11.00000  0.05    0.16
Q13   1   0.0230 -0.2419  0.5000  10.50000  0.05    0.15
Q14   1   0.0956  0.0473  0.1885  11.00000  0.05    0.14
Q15   1  -0.0148  0.2060  0.3658  11.00000  0.05    0.14
Q16   1   0.1071  0.2446  0.3529  11.00000  0.05    0.14
Q17   1   0.0967  0.3685  0.5000  10.50000  0.05    0.14
Q18   1   0.2142  0.2285  0.3144  11.00000  0.05    0.14
Q19   1   0.1897  0.4279  0.5000  10.50000  0.05    0.14
Q20   1   0.0029  0.2703  0.2711  11.00000  0.05    0.13

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0543 for 460 Fo > 4sig(Fo) and 0.0583 for all 493 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.26, deepest hole -0.23
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0583
  REM R1_gt = 0.0543
  REM wR_ref = 0.1185
  REM GOOF = 1.143
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 493
  REM Reflections_gt = 460
  REM Parameters = n/a
  REM Hole = -0.23
  REM Peak = 0.26
  REM Flack = n/a

  
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 9.928
_oxdiff_exptl_absorpt_empirical_full_min 0.723
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.755(10)
2 0.122(6)
3 -0.002(3)
4 0.125(7)

