# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_compound_2_2Py
_database_code_depnum_ccdc_archive 'CCDC 2081210'
loop_
_audit_author_name
_audit_author_address
'Hans-Georg Stammler'
;University of Bielefeld, Department of Chemistry, Inorganic and Structural Chemistry
Germany
;
_audit_update_record             
;
2021-04-30 deposited with the CCDC.	2022-04-14 downloaded from the CCDC.
;


# was schaefer12

_audit_creation_date             2020-08-06
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
?
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C20 H36 N2 Si3, 2(C F3 O3 S), C H2 Cl2'
_chemical_formula_sum            'C23 H38 Cl2 F6 N2 O6 S2 Si3'
_chemical_formula_weight         771.84
_chemical_melting_point          ?
_chemical_oxdiff_formula         C23H38Cl2F6N2O6S2Si3
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'
Cl Cl 0.3639 0.7018 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   25.5005(7)
_cell_length_b                   10.5126(2)
_cell_length_c                   29.3823(7)
_cell_angle_alpha                90
_cell_angle_beta                 113.808(3)
_cell_angle_gamma                90
_cell_volume                     7206.4(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    12519
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.3090
_cell_measurement_theta_min      3.2440
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.283
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3200
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 1 0.0512
-1 0 -1 0.0512
-1 -2 -1 0.0697
1 2 1 0.0697
2 0 -5 0.0751
-2 0 5 0.0751
5 -2 -1 0.1022
-5 2 1 0.1110
5 0 -1 0.0837

_exptl_crystal_size_max          0.208
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.102
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.9966 -0.0005 1.0015 -0.0718 -0.0320 0.0670
-0.9966 0.0005 -1.0015 0.0718 0.0320 -0.0670
-1.0058 -1.9999 -0.9955 -0.1053 0.2490 -0.1531
1.0058 1.9999 0.9955 0.1053 -0.2490 0.1531
2.0086 -0.0011 -4.9927 -0.0091 -0.1032 -0.2411
-2.0086 0.0011 4.9927 0.0091 0.1032 0.2411
4.9870 -2.0032 -0.9827 -0.4207 0.0234 -0.0727
-4.9870 2.0032 0.9827 0.4207 -0.0234 0.0727
4.9962 -0.0027 -0.9887 -0.2436 -0.1936 0.0135

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            29113
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.448
_diffrn_reflns_theta_min         3.288
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_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   -115.00  -5.00   1.00    1.00    --  -38.50 -19.00-150.00  110
  2  ω    -50.00  -6.00   1.00    1.00    --  -38.50 125.00 120.00   44
  3  ω    -46.00  33.00   1.00    1.00    --  -38.50  38.00  30.00   79
  4  ω     56.00  81.00   1.00    1.00    --   42.70 -99.00 120.00   25
  5  ω      6.00  32.00   1.00    1.00    --   42.70 -99.00 120.00   26
  6  ω     40.00  86.00   1.00    1.00    --   42.70-125.00 120.00   46
  7  ω     41.00  92.00   1.00    1.00    --   42.70-125.00 -60.00   51
  8  ω     45.00  83.00   1.00    3.00    --  111.00 -45.00-150.00   38
  9  ω     52.00 107.00   1.00    3.00    --  111.00 -94.00  60.00   55
 10  ω     44.00 121.00   1.00    3.00    --  111.00 -61.00  60.00   77
 11  ω     79.00 125.00   1.00    3.00    --  111.00 -61.00 -90.00   46
 12  ω    113.00 150.00   1.00    3.00    --  111.00  45.00 150.00   37
 13  ω     44.00  70.00   1.00    3.00    --  111.00-125.00 150.00   26
 14  ω     94.00 131.00   1.00    3.00    --  111.00 -45.00-150.00   37
 15  ω     47.00  84.00   1.00    3.00    --  111.00-125.00-120.00   37
 16  ω     37.00 102.00   1.00    3.00    --  111.00 -94.00-120.00   65
 17  ω     88.00 113.00   1.00    3.00    --  111.00-125.00-180.00   25
 18  ω     36.00 149.00   1.00    3.00    --  111.00 -15.00 120.00  113
 19  ω     43.00  69.00   1.00    3.00    --  111.00-125.00-180.00   26
 20  ω     77.00 106.00   1.00    3.00    --  111.00 -94.00   0.00   29
 21  ω     90.00 176.00   1.00    3.00    --  111.00  30.00 120.00   86
 22  ω     88.00 113.00   1.00    3.00    --  111.00-125.00 150.00   25
 23  ω     38.00 132.00   1.00    3.00    --  111.00 -30.00 -60.00   94
 24  ω     38.00  63.00   1.00    3.00    --  111.00 -94.00-180.00   25
 25  ω     66.00 107.00   1.00    3.00    --  111.00 -94.00-180.00   41
 26  ω     35.00 107.00   1.00    3.00    --  111.00-102.00 -49.46   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0525420500
_diffrn_orient_matrix_UB_12      0.0887148500
_diffrn_orient_matrix_UB_13      -0.0193451000
_diffrn_orient_matrix_UB_21      -0.0377180500
_diffrn_orient_matrix_UB_22      -0.1082928500
_diffrn_orient_matrix_UB_23      0.0055231000
_diffrn_orient_matrix_UB_31      0.0133359000
_diffrn_orient_matrix_UB_32      0.0431520000
_diffrn_orient_matrix_UB_33      0.0536485000
_diffrn_oxdiff_digest_frames     
;
0101830bfa2898784e6343c3eb8e371a9901391a08b
;
_diffrn_oxdiff_digest_hkl        
;
018b5c1049b8d01f5dd8842a33301e25b2327a
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\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                6621
_reflns_number_total             7471
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (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         0.842
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         7471
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0615
_refine_ls_restrained_S_all      1.092
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0736P)²+27.4795P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1638
_refine_ls_wR_factor_ref         0.1691
_refine_special_details          
'Disorder of oxygen and fluorine of one SO3CF3 anion over two sites in a ratio 83:17. Displacement parameters were constraint with EADP. Disorder of solvent CH2Cl2 over two sites in a ratio of 91:9. Bondlength were restrained with SADI be to become equal, the displacement parameters were constrained with EADP.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl2B-C23B \\sim Cl1A-C23A \\sim Cl2A-C23A \\sim Cl1B-C23B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C23B) = Uanis(C23A)
Uanis(O4B) = Uanis(O4A)
Uanis(O6B) = Uanis(O6A)
Uanis(O5A) = Uanis(O5B)
Uanis(F4A) = Uanis(F4B)
Uanis(F5B) = Uanis(F5A)
Uanis(F6A) = Uanis(F6B)
Uanis(Cl2A) = Uanis(Cl1B)
Uanis(Cl2B) = Uanis(Cl1A)
4. Others
 Sof(Cl1B)=Sof(Cl2B)=Sof(C23B)=Sof(H23C)=Sof(H23D)=1-FVAR(1)
 Sof(Cl1A)=Sof(Cl2A)=Sof(C23A)=Sof(H23A)=Sof(H23B)=FVAR(1)
 Sof(F4B)=Sof(F5B)=Sof(F6B)=Sof(O4B)=Sof(O5B)=Sof(O6B)=1-FVAR(2)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(O4A)=Sof(O5A)=Sof(O6A)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C7(H7A,H7B), C8(H8A,H8B), C23A(H23A,H23B),
 C23B(H23C,H23D)
5.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C9(H9A,
 H9B,H9C), C10(H10A,H10B,H10C)
;
_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
Cl1A Cl 0.50667(8) 0.20197(17) 0.58095(9) 0.0946(6) Uani 0.929(2) 1 d D . P A 1
Cl1B Cl 0.4827(6) 0.1627(15) 0.4937(5) 0.0534(3) Uani 0.071(2) 1 d D . P A 2
Cl2A Cl 0.51628(4) -0.07147(12) 0.56924(4) 0.0534(3) Uani 0.929(2) 1 d D . P A
1
Cl2B Cl 0.5248(10) 0.141(2) 0.6091(12) 0.0946(6) Uani 0.071(2) 1 d D . P A 2
S1 S 0.60126(4) 0.50822(8) 0.68737(3) 0.03422(19) Uani 1 1 d . . . . .
S2 S 0.84846(3) 0.50121(7) 0.60468(3) 0.03235(19) Uani 1 1 d . . . . .
Si1 Si 0.69582(3) 0.03476(8) 0.74955(3) 0.02748(19) Uani 1 1 d . . . . .
Si2 Si 0.69093(3) 0.01002(8) 0.59163(3) 0.02837(19) Uani 1 1 d . . . . .
Si3 Si 0.88715(3) -0.00835(8) 0.65775(3) 0.02572(18) Uani 1 1 d . . . . .
F1 F 0.55304(12) 0.4865(3) 0.59035(9) 0.0740(9) Uani 1 1 d . . . . .
F2 F 0.58528(15) 0.6726(3) 0.61649(12) 0.0813(9) Uani 1 1 d . . . . .
F3 F 0.64342(11) 0.5182(3) 0.61957(10) 0.0723(9) Uani 1 1 d . . . . .
F4A F 0.75695(16) 0.3591(4) 0.5727(3) 0.0853(17) Uani 0.832(10) 1 d . . P B 1
F4B F 0.7590(10) 0.366(2) 0.5464(13) 0.0853(17) Uani 0.168(10) 1 d . . P B 2
F5A F 0.74117(17) 0.5559(6) 0.58463(16) 0.0615(12) Uani 0.832(10) 1 d . . P B 1
F5B F 0.7382(11) 0.499(3) 0.5828(10) 0.0615(12) Uani 0.168(10) 1 d . . P B 2
F6A F 0.7570(2) 0.5023(6) 0.52054(18) 0.0603(13) Uani 0.832(10) 1 d . . P B 1
F6B F 0.7598(14) 0.549(3) 0.5249(11) 0.0603(13) Uani 0.168(10) 1 d . . P B 2
O1 O 0.54508(12) 0.5417(3) 0.68480(11) 0.0489(6) Uani 1 1 d . . . . .
O2 O 0.64780(11) 0.5879(3) 0.71877(10) 0.0457(6) Uani 1 1 d . . . . .
O3 O 0.61356(13) 0.3756(3) 0.69215(12) 0.0564(7) Uani 1 1 d . . . . .
O4A O 0.8593(2) 0.6312(5) 0.5961(2) 0.0564(13) Uani 0.832(10) 1 d . . P B 1
O4B O 0.8455(13) 0.632(3) 0.6070(13) 0.0564(13) Uani 0.168(10) 1 d . . P B 2
O5A O 0.87551(18) 0.4099(5) 0.58482(18) 0.0477(11) Uani 0.832(10) 1 d . . P B 1
O5B O 0.8732(11) 0.454(2) 0.5720(10) 0.0477(11) Uani 0.168(10) 1 d . . P B 2
O6A O 0.85610(17) 0.4722(6) 0.65549(17) 0.0528(12) Uani 0.832(10) 1 d . . P B 1
O6B O 0.8525(10) 0.429(3) 0.6415(9) 0.0528(12) Uani 0.168(10) 1 d . . P B 2
N1 N 0.61777(11) -0.0007(2) 0.72755(10) 0.0278(5) Uani 1 1 d . . . . .
N2 N 0.89623(11) 0.0136(2) 0.59876(10) 0.0289(5) Uani 1 1 d . . . . .
C1 C 0.70934(16) 0.1720(3) 0.79246(13) 0.0386(7) Uani 1 1 d . . . . .
H1A H 0.691439 0.246646 0.773850 0.058 Uiso 1 1 calc GR . . . .
H1B H 0.749883 0.185943 0.809205 0.058 Uiso 1 1 calc GR . . . .
H1C H 0.693709 0.154487 0.816552 0.058 Uiso 1 1 calc GR . . . .
C2 C 0.73220(14) -0.1121(3) 0.78039(13) 0.0348(7) Uani 1 1 d . . . . .
H2A H 0.722407 -0.130461 0.808006 0.052 Uiso 1 1 calc GR . . . .
H2B H 0.772922 -0.101150 0.792120 0.052 Uiso 1 1 calc GR . . . .
H2C H 0.720239 -0.181342 0.757123 0.052 Uiso 1 1 calc GR . . . .
C3 C 0.70354(14) 0.0749(3) 0.69099(12) 0.0313(6) Uani 1 1 d . . . . .
H3A H 0.682615 0.152797 0.677651 0.038 Uiso 1 1 calc R . . . .
H3B H 0.743686 0.091176 0.698741 0.038 Uiso 1 1 calc R . . . .
C4 C 0.68195(13) -0.0293(3) 0.65032(11) 0.0290(6) Uani 1 1 d . . . . .
H4A H 0.641629 -0.044506 0.642130 0.035 Uiso 1 1 calc R . . . .
H4B H 0.702386 -0.107634 0.663846 0.035 Uiso 1 1 calc R . . . .
C5 C 0.64485(16) 0.1477(4) 0.55849(16) 0.0473(9) Uani 1 1 d . . . . .
H5A H 0.605220 0.124180 0.547189 0.071 Uiso 1 1 calc GR . . . .
H5B H 0.653105 0.170822 0.530462 0.071 Uiso 1 1 calc GR . . . .
H5C H 0.652572 0.218675 0.580806 0.071 Uiso 1 1 calc GR . . . .
C6 C 0.67051(15) -0.1353(4) 0.55143(13) 0.0399(8) Uani 1 1 d . . . . .
H6A H 0.698360 -0.200943 0.566314 0.060 Uiso 1 1 calc GR . . . .
H6B H 0.669195 -0.115081 0.519128 0.060 Uiso 1 1 calc GR . . . .
H6C H 0.633490 -0.164302 0.548245 0.060 Uiso 1 1 calc GR . . . .
C7 C 0.76772(12) 0.0534(3) 0.60736(12) 0.0294(6) Uani 1 1 d . . . . .
H7A H 0.772776 0.067563 0.576755 0.035 Uiso 1 1 calc R . . . .
H7B H 0.776369 0.132557 0.625926 0.035 Uiso 1 1 calc R . . . .
C8 C 0.81037(13) -0.0493(3) 0.63813(12) 0.0308(6) Uani 1 1 d . . . . .
H8A H 0.802634 -0.126984 0.618679 0.037 Uiso 1 1 calc R . . . .
H8B H 0.803430 -0.066776 0.667646 0.037 Uiso 1 1 calc R . . . .
C9 C 0.90747(16) 0.1448(3) 0.69071(13) 0.0390(7) Uani 1 1 d . . . . .
H9A H 0.946836 0.162999 0.697591 0.059 Uiso 1 1 calc GR . . . .
H9B H 0.902592 0.140098 0.721401 0.059 Uiso 1 1 calc GR . . . .
H9C H 0.883558 0.211086 0.670312 0.059 Uiso 1 1 calc GR . . . .
C10 C 0.93468(14) -0.1424(3) 0.68940(13) 0.0362(7) Uani 1 1 d . . . . .
H10A H 0.919147 -0.219953 0.671905 0.054 Uiso 1 1 calc GR . . . .
H10B H 0.937538 -0.148865 0.722918 0.054 Uiso 1 1 calc GR . . . .
H10C H 0.972061 -0.128057 0.689848 0.054 Uiso 1 1 calc GR . . . .
C11 C 0.59852(13) -0.1207(3) 0.72019(12) 0.0315(6) Uani 1 1 d . . . . .
H11 H 0.624829 -0.186916 0.727358 0.038 Uiso 1 1 calc R . . . .
C12 C 0.54117(14) -0.1490(3) 0.70239(13) 0.0380(7) Uani 1 1 d . . . . .
H12 H 0.528782 -0.233047 0.696874 0.046 Uiso 1 1 calc R . . . .
C13 C 0.50250(16) -0.0519(4) 0.69289(17) 0.0502(9) Uani 1 1 d . . . . .
H13 H 0.463637 -0.068970 0.682793 0.060 Uiso 1 1 calc R . . . .
C14 C 0.5219(2) 0.0706(5) 0.6985(2) 0.0734(16) Uani 1 1 d . . . . .
H14 H 0.495989 0.137685 0.690819 0.088 Uiso 1 1 calc R . . . .
C15 C 0.57979(17) 0.0951(4) 0.71544(19) 0.0567(11) Uani 1 1 d . . . . .
H15 H 0.592635 0.178732 0.718517 0.068 Uiso 1 1 calc R . . . .
C16 C 0.91325(16) 0.1253(3) 0.58668(13) 0.0408(8) Uani 1 1 d . . . . .
H16 H 0.920987 0.193107 0.608778 0.049 Uiso 1 1 calc R . . . .
C17 C 0.91952(19) 0.1423(5) 0.54287(14) 0.0538(10) Uani 1 1 d . . . . .
H17 H 0.931530 0.220191 0.535522 0.065 Uiso 1 1 calc R . . . .
C18 C 0.90806(19) 0.0448(5) 0.51067(15) 0.0561(11) Uani 1 1 d . . . . .
H18 H 0.911727 0.055204 0.480660 0.067 Uiso 1 1 calc R . . . .
C19 C 0.8911(2) -0.0692(5) 0.52206(16) 0.0607(12) Uani 1 1 d . . . . .
H19 H 0.883045 -0.136667 0.499798 0.073 Uiso 1 1 calc R . . . .
C20 C 0.88584(18) -0.0846(4) 0.56700(14) 0.0456(8) Uani 1 1 d . . . . .
H20 H 0.875098 -0.163093 0.575125 0.055 Uiso 1 1 calc R . . . .
C21 C 0.59604(17) 0.5484(4) 0.62553(14) 0.0479(9) Uani 1 1 d . . . . .
C22 C 0.77233(16) 0.4788(4) 0.56787(15) 0.0420(8) Uani 1 1 d . . . . .
C23A C 0.47043(19) 0.0603(5) 0.5539(2) 0.0594(12) Uani 0.929(2) 1 d D . P A 1
H23A H 0.439987 0.045508 0.565084 0.071 Uiso 0.929(2) 1 calc R . P A 1
H23B H 0.452998 0.069996 0.518015 0.071 Uiso 0.929(2) 1 calc R . P A 1
C23B C 0.483(3) 0.092(7) 0.5480(9) 0.0594(12) Uani 0.071(2) 1 d D . P A 2
H23C H 0.443969 0.092708 0.544640 0.071 Uiso 0.071(2) 1 calc R . P A 2
H23D H 0.493084 0.003065 0.546402 0.071 Uiso 0.071(2) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1A C23A 1.764(6) . ?
Cl1B C23B 1.756(17) . ?
Cl2A C23A 1.751(5) . ?
Cl2B C23B 1.753(17) . ?
S1 O1 1.447(3) . ?
S1 O2 1.441(3) . ?
S1 O3 1.423(3) . ?
S1 C21 1.817(4) . ?
S2 O4A 1.437(5) . ?
S2 O4B 1.38(3) . ?
S2 O5A 1.436(4) . ?
S2 O5B 1.43(2) . ?
S2 O6A 1.458(4) . ?
S2 O6B 1.29(3) . ?
S2 C22 1.816(4) . ?
Si1 N1 1.865(3) . ?
Si1 C1 1.855(3) . ?
Si1 C2 1.840(3) . ?
Si1 C3 1.858(3) . ?
Si2 C4 1.875(3) . ?
Si2 C5 1.871(4) . ?
Si2 C6 1.871(4) . ?
Si2 C7 1.878(3) . ?
Si3 N2 1.853(3) . ?
Si3 C8 1.855(3) . ?
Si3 C9 1.842(3) . ?
Si3 C10 1.847(3) . ?
F1 C21 1.334(5) . ?
F2 C21 1.338(5) . ?
F3 C21 1.327(5) . ?
F4A C22 1.342(6) . ?
F4B C22 1.32(3) . ?
F5A C22 1.359(6) . ?
F5B C22 1.14(2) . ?
F6A C22 1.307(6) . ?
F6B C22 1.38(3) . ?
N1 C11 1.339(4) . ?
N1 C15 1.342(4) . ?
N2 C16 1.349(4) . ?
N2 C20 1.344(4) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.549(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.541(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11 0.9300 . ?
C11 C12 1.372(5) . ?
C12 H12 0.9300 . ?
C12 C13 1.368(5) . ?
C13 H13 0.9300 . ?
C13 C14 1.365(7) . ?
C14 H14 0.9300 . ?
C14 C15 1.378(6) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C16 C17 1.371(5) . ?
C17 H17 0.9300 . ?
C17 C18 1.345(7) . ?
C18 H18 0.9300 . ?
C18 C19 1.360(7) . ?
C19 H19 0.9300 . ?
C19 C20 1.390(6) . ?
C20 H20 0.9300 . ?
C23A H23A 0.9700 . ?
C23A H23B 0.9700 . ?
C23B H23C 0.9700 . ?
C23B H23D 0.9700 . ?

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
O1 S1 C21 102.70(18) . . ?
O2 S1 O1 115.72(17) . . ?
O2 S1 C21 102.35(18) . . ?
O3 S1 O1 114.69(19) . . ?
O3 S1 O2 114.46(18) . . ?
O3 S1 C21 104.5(2) . . ?
O4A S2 O6A 115.0(3) . . ?
O4A S2 C22 104.7(2) . . ?
O4B S2 O5B 115.1(14) . . ?
O4B S2 C22 95.3(13) . . ?
O5A S2 O4A 114.0(2) . . ?
O5A S2 O6A 112.9(2) . . ?
O5A S2 C22 104.2(2) . . ?
O5B S2 C22 102.2(11) . . ?
O6A S2 C22 104.6(2) . . ?
O6B S2 O4B 122.1(16) . . ?
O6B S2 O5B 116.8(13) . . ?
O6B S2 C22 97.3(12) . . ?
C1 Si1 N1 105.70(15) . . ?
C1 Si1 C3 113.14(15) . . ?
C2 Si1 N1 104.97(14) . . ?
C2 Si1 C1 113.55(16) . . ?
C2 Si1 C3 115.19(15) . . ?
C3 Si1 N1 102.81(13) . . ?
C4 Si2 C7 109.25(14) . . ?
C5 Si2 C4 111.40(17) . . ?
C5 Si2 C6 110.28(19) . . ?
C5 Si2 C7 108.28(16) . . ?
C6 Si2 C4 107.12(15) . . ?
C6 Si2 C7 110.53(15) . . ?
N2 Si3 C8 104.66(13) . . ?
C9 Si3 N2 105.56(14) . . ?
C9 Si3 C8 113.83(16) . . ?
C9 Si3 C10 114.46(17) . . ?
C10 Si3 N2 105.15(14) . . ?
C10 Si3 C8 112.04(15) . . ?
C11 N1 Si1 121.0(2) . . ?
C11 N1 C15 119.1(3) . . ?
C15 N1 Si1 119.8(2) . . ?
C16 N2 Si3 122.0(2) . . ?
C20 N2 Si3 119.3(2) . . ?
C20 N2 C16 118.7(3) . . ?
Si1 C1 H1A 109.5 . . ?
Si1 C1 H1B 109.5 . . ?
Si1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si1 C3 H3A 108.6 . . ?
Si1 C3 H3B 108.6 . . ?
H3A C3 H3B 107.6 . . ?
C4 C3 Si1 114.6(2) . . ?
C4 C3 H3A 108.6 . . ?
C4 C3 H3B 108.6 . . ?
Si2 C4 H4A 108.6 . . ?
Si2 C4 H4B 108.6 . . ?
C3 C4 Si2 114.6(2) . . ?
C3 C4 H4A 108.6 . . ?
C3 C4 H4B 108.6 . . ?
H4A C4 H4B 107.6 . . ?
Si2 C5 H5A 109.5 . . ?
Si2 C5 H5B 109.5 . . ?
Si2 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
Si2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si2 C7 H7A 109.0 . . ?
Si2 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C8 C7 Si2 113.1(2) . . ?
C8 C7 H7A 109.0 . . ?
C8 C7 H7B 109.0 . . ?
Si3 C8 H8A 108.5 . . ?
Si3 C8 H8B 108.5 . . ?
C7 C8 Si3 115.2(2) . . ?
C7 C8 H8A 108.5 . . ?
C7 C8 H8B 108.5 . . ?
H8A C8 H8B 107.5 . . ?
Si3 C9 H9A 109.5 . . ?
Si3 C9 H9B 109.5 . . ?
Si3 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si3 C10 H10A 109.5 . . ?
Si3 C10 H10B 109.5 . . ?
Si3 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 H11 119.0 . . ?
N1 C11 C12 122.1(3) . . ?
C12 C11 H11 119.0 . . ?
C11 C12 H12 120.5 . . ?
C13 C12 C11 119.0(3) . . ?
C13 C12 H12 120.5 . . ?
C12 C13 H13 120.6 . . ?
C14 C13 C12 118.9(4) . . ?
C14 C13 H13 120.6 . . ?
C13 C14 H14 119.9 . . ?
C13 C14 C15 120.2(4) . . ?
C15 C14 H14 119.9 . . ?
N1 C15 C14 120.6(4) . . ?
N1 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
N2 C16 H16 118.9 . . ?
N2 C16 C17 122.1(4) . . ?
C17 C16 H16 118.9 . . ?
C16 C17 H17 120.4 . . ?
C18 C17 C16 119.1(4) . . ?
C18 C17 H17 120.4 . . ?
C17 C18 H18 120.1 . . ?
C17 C18 C19 119.9(4) . . ?
C19 C18 H18 120.1 . . ?
C18 C19 H19 120.0 . . ?
C18 C19 C20 119.9(4) . . ?
C20 C19 H19 120.0 . . ?
N2 C20 C19 120.1(4) . . ?
N2 C20 H20 119.9 . . ?
C19 C20 H20 119.9 . . ?
F1 C21 S1 111.5(3) . . ?
F1 C21 F2 106.5(4) . . ?
F2 C21 S1 110.6(3) . . ?
F3 C21 S1 111.9(3) . . ?
F3 C21 F1 106.8(3) . . ?
F3 C21 F2 109.4(4) . . ?
F4A C22 S2 110.3(3) . . ?
F4A C22 F5A 106.4(4) . . ?
F4B C22 S2 114.1(11) . . ?
F4B C22 F6B 96.9(15) . . ?
F5A C22 S2 110.3(3) . . ?
F5B C22 S2 123.0(14) . . ?
F5B C22 F4B 105.2(16) . . ?
F5B C22 F6B 108.7(19) . . ?
F6A C22 S2 113.4(3) . . ?
F6A C22 F4A 108.3(4) . . ?
F6A C22 F5A 107.7(4) . . ?
F6B C22 S2 105.8(13) . . ?
Cl1A C23A H23A 109.2 . . ?
Cl1A C23A H23B 109.2 . . ?
Cl2A C23A Cl1A 112.2(3) . . ?
Cl2A C23A H23A 109.2 . . ?
Cl2A C23A H23B 109.2 . . ?
H23A C23A H23B 107.9 . . ?
Cl1B C23B H23C 105.8 . . ?
Cl1B C23B H23D 105.8 . . ?
Cl2B C23B Cl1B 126(3) . . ?
Cl2B C23B H23C 105.8 . . ?
Cl2B C23B H23D 105.8 . . ?
H23C C23B H23D 106.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Si1 N1 C11 C12 -177.7(3) . . . . ?
Si1 N1 C15 C14 179.1(4) . . . . ?
Si1 C3 C4 Si2 -178.98(16) . . . . ?
Si2 C7 C8 Si3 -176.87(16) . . . . ?
Si3 N2 C16 C17 -179.4(3) . . . . ?
Si3 N2 C20 C19 178.5(3) . . . . ?
O1 S1 C21 F1 -57.4(3) . . . . ?
O1 S1 C21 F2 60.9(3) . . . . ?
O1 S1 C21 F3 -176.9(3) . . . . ?
O2 S1 C21 F1 -177.7(3) . . . . ?
O2 S1 C21 F2 -59.4(3) . . . . ?
O2 S1 C21 F3 62.8(4) . . . . ?
O3 S1 C21 F1 62.7(3) . . . . ?
O3 S1 C21 F2 -179.1(3) . . . . ?
O3 S1 C21 F3 -56.9(4) . . . . ?
O4A S2 C22 F4A 179.6(4) . . . . ?
O4A S2 C22 F5A -63.1(4) . . . . ?
O4A S2 C22 F6A 57.9(4) . . . . ?
O4B S2 C22 F4B 163.3(17) . . . . ?
O4B S2 C22 F5B -67.4(19) . . . . ?
O4B S2 C22 F6B 58.1(18) . . . . ?
O5A S2 C22 F4A 59.6(4) . . . . ?
O5A S2 C22 F5A 176.9(3) . . . . ?
O5A S2 C22 F6A -62.1(4) . . . . ?
O5B S2 C22 F4B 46.2(15) . . . . ?
O5B S2 C22 F5B 175.5(17) . . . . ?
O5B S2 C22 F6B -59.1(16) . . . . ?
O6A S2 C22 F4A -59.1(4) . . . . ?
O6A S2 C22 F5A 58.2(4) . . . . ?
O6A S2 C22 F6A 179.2(4) . . . . ?
O6B S2 C22 F4B -73.3(15) . . . . ?
O6B S2 C22 F5B 55.9(18) . . . . ?
O6B S2 C22 F6B -178.6(16) . . . . ?
N1 Si1 C3 C4 -55.8(2) . . . . ?
N1 C11 C12 C13 -1.5(5) . . . . ?
N2 Si3 C8 C7 -61.4(3) . . . . ?
N2 C16 C17 C18 0.4(6) . . . . ?
C1 Si1 N1 C11 -143.0(3) . . . . ?
C1 Si1 N1 C15 41.9(4) . . . . ?
C1 Si1 C3 C4 -169.3(2) . . . . ?
C2 Si1 N1 C11 -22.6(3) . . . . ?
C2 Si1 N1 C15 162.2(3) . . . . ?
C2 Si1 C3 C4 57.8(3) . . . . ?
C3 Si1 N1 C11 98.2(3) . . . . ?
C3 Si1 N1 C15 -77.0(3) . . . . ?
C4 Si2 C7 C8 54.5(3) . . . . ?
C5 Si2 C4 C3 -66.0(3) . . . . ?
C5 Si2 C7 C8 176.0(2) . . . . ?
C6 Si2 C4 C3 173.3(2) . . . . ?
C6 Si2 C7 C8 -63.1(3) . . . . ?
C7 Si2 C4 C3 53.6(3) . . . . ?
C8 Si3 N2 C16 119.0(3) . . . . ?
C8 Si3 N2 C20 -61.3(3) . . . . ?
C9 Si3 N2 C16 -1.4(3) . . . . ?
C9 Si3 N2 C20 178.3(3) . . . . ?
C9 Si3 C8 C7 53.3(3) . . . . ?
C10 Si3 N2 C16 -122.8(3) . . . . ?
C10 Si3 N2 C20 56.9(3) . . . . ?
C10 Si3 C8 C7 -174.8(2) . . . . ?
C11 N1 C15 C14 3.9(7) . . . . ?
C11 C12 C13 C14 4.0(7) . . . . ?
C12 C13 C14 C15 -2.7(8) . . . . ?
C13 C14 C15 N1 -1.3(9) . . . . ?
C15 N1 C11 C12 -2.5(5) . . . . ?
C16 N2 C20 C19 -1.8(6) . . . . ?
C16 C17 C18 C19 -0.7(7) . . . . ?
C17 C18 C19 C20 -0.2(7) . . . . ?
C18 C19 C20 N2 1.5(7) . . . . ?
C20 N2 C16 C17 0.9(5) . . . . ?

_olex2_date_sample_data_collection 2020-08-06
_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 1.230
_oxdiff_exptl_absorpt_empirical_full_min 0.813
####################################################################### 
# 
# 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_compound_2_Bipy
_database_code_depnum_ccdc_archive 'CCDC 2081211'
loop_
_audit_author_name
_audit_author_address
'Hans-Georg Stammler'
;University of Bielefeld, Department of Chemistry, Inorganic and Structural Chemistry
Germany
;
_audit_update_record             
;
2021-04-30 deposited with the CCDC.	2022-04-14 downloaded from the CCDC.
;


# was schaefer16_twin1_hklf4

_audit_creation_date             2020-10-22
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
?
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C40 H68 N4 Si6, 4(C F3 O3 S), 3(C2 H3 N)'
_chemical_formula_sum            'C50 H77 F12 N7 O12 S4 Si6'
_chemical_formula_weight         1492.96
_chemical_melting_point          ?
_chemical_oxdiff_formula         C48H66F10N6O12S4Si6
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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.5131(7)
_cell_length_b                   13.0673(6)
_cell_length_c                   13.5178(6)
_cell_angle_alpha                115.737(4)
_cell_angle_beta                 101.219(4)
_cell_angle_gamma                107.630(4)
_cell_volume                     1755.33(16)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    10762
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.3500
_cell_measurement_theta_min      3.8440
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.024
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.730
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             778
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 0 2 0.0267
5 0 -2 0.0267
3 -2 -5 0.0601
-3 2 5 0.0391
0 -4 5 0.0529
0 4 -5 0.0529

_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.053
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-4.9912 0.0077 2.0006 0.4591 0.1098 0.4389
4.9912 -0.0077 -2.0006 -0.4591 -0.1098 -0.4389
2.9549 -1.9919 -4.9809 -0.4293 -0.6356 0.1420
-2.9549 1.9919 4.9809 0.4293 0.6356 -0.1420
0.0310 -3.9839 4.9742 0.5269 -0.1255 -0.2994
-0.0310 3.9839 -4.9742 -0.5269 0.1255 0.2994

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_number            27959
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.242
_diffrn_reflns_theta_min         3.924
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -106.00  -6.00   1.00    3.08    --  -38.05 -57.00 -60.00  100
  2  ω    -47.00  -9.00   1.00    3.08    --  -38.05 -57.00   0.00   38
  3  ω    -53.00 -13.00   1.00    3.08    --  -38.05 -57.00-120.00   40
  4  ω   -127.00 -72.00   1.00    3.08    --  -38.05-178.00 150.00   55
  5  ω   -112.00 -41.00   1.00    3.08    --  -38.05 -57.00 -90.00   71
  6  ω    -91.00  -6.00   1.00    3.08    --  -38.05 -57.00 120.00   85
  7  ω   -114.00 -43.00   1.00    3.08    --  -38.05 178.00 -30.00   71
  8  ω   -127.00  23.00   1.00    3.08    --  -38.05   0.00  30.00  150
  9  ω    -63.00  40.00   1.00    3.08    --  -38.05  38.00-180.00  103
 10  ω   -116.00  -6.00   1.00    3.08    --  -38.05 -57.00  30.00  110
 11  ω    -73.00  -9.00   1.00    3.08    --  -38.05 -38.00 120.00   64
 12  ω   -123.00 -38.00   1.00    3.08    --  -38.05 178.00 -60.00   85
 13  ω    -89.00 -40.00   1.00    3.08    --  -38.05 -38.00  30.00   49
 14  ω   -113.00 -86.00   1.00    3.08    --  -38.05 -57.00   0.00   27
 15  ω   -114.00 -62.00   1.00    3.08    --  -38.05 -57.00-120.00   52
 16  ω      6.00  35.00   1.00    3.08    --   38.05 -99.00   0.00   29
 17  ω     75.00 100.00   1.00    3.08    --   38.05  57.00 -90.00   25
 18  ω      6.00  68.00   1.00    3.08    --   38.05  57.00 -90.00   62
 19  ω     56.00  82.00   1.00    3.08    --   38.05 -99.00   0.00   26
 20  ω     -1.00  26.00   1.00    3.08    --   38.05  89.00 166.72   27
 21  ω     30.00  76.00   1.00    3.08    --   38.05 -99.00-180.00   46
 22  ω     59.00 114.00   1.00    3.08    --   38.05-178.00 -30.00   55
 23  ω     -3.00  23.00   1.00    3.08    --   38.05  92.00  10.34   26
 24  ω     18.00 117.00   1.00    3.08    --   38.05  19.00-150.00   99
 25  ω      3.00  32.00   1.00    3.08    --   38.05  77.00 -72.59   29
 26  ω     79.00 108.00   1.00    3.08    --   38.05 178.00  60.00   29
 27  ω     35.00 108.00   1.00   13.50    --  115.00-111.00 -90.00   73
 28  ω     81.00 110.00   1.00   13.50    --  115.00  62.00  98.48   29
 29  ω     82.00 110.00   1.00   13.50    --  115.00  61.00  60.00   28
 30  ω     82.00 110.00   1.00   13.50    --  115.00  61.00-120.00   28
 31  ω    127.00 175.00   1.00   13.50    --  115.00  61.00  90.00   48
 32  ω     83.00 110.00   1.00   13.50    --  115.00  53.00 141.01   27
 33  ω     84.00 113.00   1.00   13.50    --  115.00  45.00  73.17   29
 34  ω     31.00 106.00   1.00   13.50    --  115.00 -94.00  60.00   75
 35  ω     33.00  93.00   1.00   13.50    --  115.00 -77.00   0.00   60
 36  ω    117.00 178.00   1.00   13.50    --  115.00  66.00 -97.58   61
 37  ω     84.00 111.00   1.00   13.50    --  115.00  45.00   0.00   27
 38  ω     85.00 110.00   1.00   13.50    --  115.00  45.00  60.00   25
 39  ω     80.00 108.00   1.00   13.50    --  115.00  66.00 -97.58   28
 40  ω     84.00 178.00   1.00   13.50    --  115.00  33.00-174.51   94
 41  ω     79.00 107.00   1.00   13.50    --  115.00  65.00 162.43   28
 42  ω    131.00 178.00   1.00   13.50    --  115.00  61.00 120.00   47
 43  ω     29.00 107.00   1.00   13.50    --  115.00 -94.00-180.00   78
 44  ω     83.00 126.00   1.00   13.50    --  115.00  61.00 120.00   43
 45  ω     34.00  86.00   1.00   13.50    --  115.00-111.00-120.00   52
 46  ω     82.00 158.00   1.00   13.50    --  115.00  61.00 -60.00   76
 47  ω    120.00 178.00   1.00   13.50    --  115.00  70.00  62.60   58
 48  ω     80.00 110.00   1.00   13.50    --  115.00  63.00   7.73   30
 49  ω     82.00 112.00   1.00   13.50    --  115.00  61.00-180.00   30
 50  ω     77.00 109.00   1.00   13.50    --  115.00  30.00 -60.00   32
 51  ω     43.00 109.00   1.00   13.50    --  115.00-111.00   0.00   66
 52  ω    108.00 150.00   1.00   13.50    --  115.00 -77.00   0.00   42
 53  ω     85.00 111.00   1.00   13.50    --  115.00  45.00-150.00   26
 54  ω     82.00 117.00   1.00   13.50    --  115.00  61.00  90.00   35
 55  ω     80.00 156.00   1.00   13.50    --  115.00  64.00 -46.28   76
 56  ω     80.00 109.00   1.00   13.50    --  115.00  66.00 136.89   29
 57  ω     80.00 115.00   1.00   13.50    --  115.00  70.00  62.60   35
 58  ω     83.00 157.00   1.00   13.50    --  115.00  52.00   6.04   74
 59  ω     31.00  86.00   1.00   13.50    --  115.00 -77.00 -90.00   55
 60  ω     86.00 115.00   1.00   13.50    --  115.00  45.00-120.00   29
 61  ω    150.00 175.00   1.00   13.50    --  115.00  51.00-147.66   25
 62  ω    134.00 162.00   1.00   13.50    --  115.00  61.00-120.00   28
 63  ω     73.00 107.00   1.00   13.50    --  115.00 -94.00 120.00   34
 64  ω     29.00  58.00   1.00   13.50    --  115.00 -94.00 120.00   29
 65  ω     83.00 120.00   1.00   13.50    --  115.00  51.00-147.66   37
 66  ω     84.00 129.00   1.00   13.50    --  115.00  44.00 101.73   45
 67  ω     83.00 112.00   1.00   13.50    --  115.00  61.00 150.00   29
 68  ω     82.00 176.00   1.00   13.50    --  115.00  61.00  30.00   94
 69  ω     84.00  96.00   1.00   13.50    --  115.00  54.00 112.88   12
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0651592000
_diffrn_orient_matrix_UB_12      -0.0489658000
_diffrn_orient_matrix_UB_13      0.0671171000
_diffrn_orient_matrix_UB_21      0.0106360000
_diffrn_orient_matrix_UB_22      0.1325804000
_diffrn_orient_matrix_UB_23      0.0808970000
_diffrn_orient_matrix_UB_31      -0.1230573000
_diffrn_orient_matrix_UB_32      -0.0350581000
_diffrn_orient_matrix_UB_33      -0.0874981000
_diffrn_oxdiff_digest_frames     
;
011194f140eafd0171889f1edab3dcef0d000288ac0
;
_diffrn_oxdiff_digest_hkl        
;
01b04f589c3e2bd21d5a1958e11f19f7f962f2
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\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                7365
_reflns_number_total             10019
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_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         0.573
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         10019
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0590
_refine_ls_restrained_S_all      1.055
_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)+(0.1183P)²+0.0513P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1638
_refine_ls_wR_factor_ref         0.1768
_refine_special_details          
'Twinned crystal (63:37). Component 2 rotated by 2.6745 deg. around [-0.44 0.52 0.74] (reciprocal) or [0.07 0.680.73] (direct). Disorder of one Trifluormethansulfonat over two sites (54:46). Disorder of acetronitrile on an inversion center. Bondlength were restrained with SADI to become equal with those of the second acetronitrile.,Twin'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.627(3)
 0.373(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N3-C21 \\sim N4-C25
 with sigma of 0.02
 C22-C21 \\sim C26-C25
 with sigma of 0.02
4. Others
 Sof(S2B)=Sof(F4B)=Sof(O4B)=Sof(C24B)=1-FVAR(1)
 Sof(S2)=Sof(F4)=Sof(O4)=Sof(C24)=FVAR(1)
 Fixed Sof: N4(0.5) C25(0.5) C26(0.5) H26A(0.5) H26B(0.5) H26C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C7(H7A,H7B), C8(H8A,H8B)
5.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20)
5.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C5(H5A,H5B,H5C),
 C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C22(H22A,H22B,H22C)
;
_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
S1 S 0.78933(8) 0.75022(8) 1.17010(7) 0.0401(2) Uani 1 1 d . . . . .
S2 S 0.37521(13) 0.10536(14) 0.30827(12) 0.0316(4) Uani 0.541(3) 1 d . . P A 1
S2B S 0.36476(16) 0.01766(16) 0.27005(15) 0.0332(5) Uani 0.459(3) 1 d . . P A 2
Si1 Si 0.58624(8) 0.27911(7) 0.07083(7) 0.0308(2) Uani 1 1 d . . . . .
Si2 Si 0.93681(8) 0.27967(8) 0.24701(8) 0.0345(2) Uani 1 1 d . . . . .
Si3 Si 0.75546(8) 0.09281(7) 0.42875(7) 0.0327(2) Uani 1 1 d . . . . .
F1 F 0.8143(3) 0.8082(3) 1.0106(3) 0.0707(8) Uani 1 1 d . . . . .
F2 F 0.7753(2) 0.6139(3) 0.9541(2) 0.0638(7) Uani 1 1 d . . . . .
F3 F 0.9535(2) 0.7628(3) 1.0740(2) 0.0676(7) Uani 1 1 d . . . . .
F4 F 0.2211(4) -0.1321(3) 0.1575(4) 0.0501(10) Uani 0.541(3) 1 d . . P A 1
F4B F 0.2805(5) 0.1814(4) 0.2867(5) 0.0483(12) Uani 0.459(3) 1 d . . P A 2
F5 F 0.14425(19) -0.0049(2) 0.2464(2) 0.0522(5) Uani 1 1 d . . . . .
F6 F 0.1984(2) 0.0055(3) 0.1085(2) 0.0599(6) Uani 1 1 d . . . . .
O1 O 0.8191(3) 0.6647(2) 1.1968(3) 0.0561(7) Uani 1 1 d . . . . .
O2 O 0.8602(3) 0.8822(2) 1.2610(3) 0.0546(7) Uani 1 1 d . . . . .
O3 O 0.6613(3) 0.7104(3) 1.1185(3) 0.0496(6) Uani 1 1 d . . . . .
O4 O 0.3603(5) 0.2200(4) 0.3499(4) 0.0380(10) Uani 0.541(3) 1 d . . P A 1
O4B O 0.3099(6) -0.1182(5) 0.2015(5) 0.0457(13) Uani 0.459(3) 1 d . . P A 2
O5 O 0.3946(2) 0.0704(2) 0.3953(2) 0.0407(5) Uani 1 1 d . . . . .
O6 O 0.4544(2) 0.0881(3) 0.2401(2) 0.0452(6) Uani 1 1 d . . . . .
N1 N 0.7029(2) 0.2100(2) 0.5150(2) 0.0300(5) Uani 1 1 d . . . . .
N2 N 0.4761(2) 0.6164(2) 0.8418(2) 0.0303(5) Uani 1 1 d . . . . .
N3 N 0.2713(4) 0.4384(4) 0.5469(4) 0.0662(11) Uani 1 1 d D . . . .
N4 N 0.909(2) 0.423(2) 0.896(2) 0.111(8) Uani 0.5 1 d D . P B -1
C25 C 0.9768(16) 0.498(3) 0.989(2) 0.067(5) Uani 0.5 1 d D . P B -1
C26 C 1.0699(19) 0.5992(19) 1.1087(16) 0.061(3) Uani 0.5 1 d D . P B -1
H26A H 1.120930 0.567200 1.136003 0.092 Uiso 0.5 1 calc GR . P B -1
H26B H 1.031046 0.627201 1.162892 0.092 Uiso 0.5 1 calc GR . P B -1
H26C H 1.118265 0.668822 1.104525 0.092 Uiso 0.5 1 calc GR . P B -1
C1 C 0.4593(3) 0.1195(3) -0.0145(3) 0.0380(7) Uani 1 1 d . . . . .
H1A H 0.439585 0.094236 0.039104 0.057 Uiso 1 1 calc GR . . . .
H1B H 0.482255 0.060951 -0.067799 0.057 Uiso 1 1 calc GR . . . .
H1C H 0.389967 0.120036 -0.059139 0.057 Uiso 1 1 calc GR . . . .
C2 C 0.6326(3) 0.3363(3) -0.0243(3) 0.0404(7) Uani 1 1 d . . . . .
H2A H 0.566423 0.342150 -0.067400 0.061 Uiso 1 1 calc GR . . . .
H2B H 0.654787 0.278246 -0.079201 0.061 Uiso 1 1 calc GR . . . .
H2C H 0.700753 0.418084 0.024329 0.061 Uiso 1 1 calc GR . . . .
C3 C 0.7180(3) 0.3067(3) 0.1860(3) 0.0362(7) Uani 1 1 d . . . . .
H3A H 0.770792 0.396633 0.235846 0.043 Uiso 1 1 calc R . . . .
H3B H 0.689670 0.278660 0.235767 0.043 Uiso 1 1 calc R . . . .
C4 C 0.7916(3) 0.2369(3) 0.1329(3) 0.0343(6) Uani 1 1 d . . . . .
H4A H 0.810510 0.256240 0.075027 0.041 Uiso 1 1 calc R . . . .
H4B H 0.741767 0.146483 0.091600 0.041 Uiso 1 1 calc R . . . .
C5 C 1.0069(4) 0.1738(4) 0.1801(4) 0.0499(9) Uani 1 1 d . . . . .
H5A H 0.956381 0.089537 0.158154 0.075 Uiso 1 1 calc GR . . . .
H5B H 1.085441 0.203597 0.236844 0.075 Uiso 1 1 calc GR . . . .
H5C H 1.014953 0.173673 0.110909 0.075 Uiso 1 1 calc GR . . . .
C6 C 1.0433(4) 0.4478(4) 0.3106(4) 0.0544(10) Uani 1 1 d . . . . .
H6A H 1.064941 0.456924 0.249555 0.082 Uiso 1 1 calc GR . . . .
H6B H 1.114968 0.471917 0.373189 0.082 Uiso 1 1 calc GR . . . .
H6C H 1.004712 0.500976 0.341745 0.082 Uiso 1 1 calc GR . . . .
C7 C 0.8996(3) 0.2623(3) 0.3690(3) 0.0331(6) Uani 1 1 d . . . . .
H7A H 0.971154 0.273325 0.423698 0.040 Uiso 1 1 calc R . . . .
H7B H 0.877005 0.328196 0.412797 0.040 Uiso 1 1 calc R . . . .
C8 C 0.7949(3) 0.1318(3) 0.3204(3) 0.0324(6) Uani 1 1 d . . . . .
H8A H 0.815181 0.067408 0.269458 0.039 Uiso 1 1 calc R . . . .
H8B H 0.722808 0.125367 0.270807 0.039 Uiso 1 1 calc R . . . .
C9 C 0.6216(3) -0.0601(3) 0.3574(3) 0.0419(8) Uani 1 1 d . . . . .
H9A H 0.605117 -0.076128 0.417040 0.063 Uiso 1 1 calc GR . . . .
H9B H 0.637037 -0.126300 0.303798 0.063 Uiso 1 1 calc GR . . . .
H9C H 0.552791 -0.057628 0.314083 0.063 Uiso 1 1 calc GR . . . .
C10 C 0.8856(3) 0.1153(3) 0.5409(3) 0.0413(7) Uani 1 1 d . . . . .
H10A H 0.944698 0.202123 0.585173 0.062 Uiso 1 1 calc GR . . . .
H10B H 0.921254 0.062086 0.502106 0.062 Uiso 1 1 calc GR . . . .
H10C H 0.858473 0.093574 0.593892 0.062 Uiso 1 1 calc GR . . . .
C11 C 0.6900(4) 0.2199(3) 0.6151(3) 0.0448(8) Uani 1 1 d . . . . .
H11 H 0.711475 0.171348 0.641455 0.054 Uiso 1 1 calc R . . . .
C12 C 0.6461(4) 0.2993(3) 0.6793(3) 0.0428(8) Uani 1 1 d . . . . .
H12 H 0.638265 0.304335 0.748054 0.051 Uiso 1 1 calc R . . . .
C13 C 0.6132(3) 0.3727(3) 0.6404(3) 0.0300(6) Uani 1 1 d . . . . .
C14 C 0.6266(3) 0.3618(3) 0.5380(3) 0.0342(6) Uani 1 1 d . . . . .
H14 H 0.605643 0.409326 0.509735 0.041 Uiso 1 1 calc R . . . .
C15 C 0.6711(3) 0.2804(3) 0.4778(3) 0.0335(6) Uani 1 1 d . . . . .
H15 H 0.679533 0.273719 0.408702 0.040 Uiso 1 1 calc R . . . .
C16 C 0.5405(3) 0.6484(3) 0.7818(3) 0.0336(6) Uani 1 1 d . . . . .
H16 H 0.554851 0.724607 0.786089 0.040 Uiso 1 1 calc R . . . .
C17 C 0.5855(3) 0.5722(3) 0.7148(3) 0.0336(6) Uani 1 1 d . . . . .
H17 H 0.629685 0.596527 0.674545 0.040 Uiso 1 1 calc R . . . .
C18 C 0.5639(3) 0.4568(3) 0.7080(3) 0.0293(6) Uani 1 1 d . . . . .
C19 C 0.4944(3) 0.4236(3) 0.7669(3) 0.0322(6) Uani 1 1 d . . . . .
H19 H 0.475941 0.346350 0.761354 0.039 Uiso 1 1 calc R . . . .
C20 C 0.4526(3) 0.5045(3) 0.8337(3) 0.0340(6) Uani 1 1 d . . . . .
H20 H 0.407293 0.481718 0.873970 0.041 Uiso 1 1 calc R . . . .
C21 C 0.2396(4) 0.3404(4) 0.5324(3) 0.0460(8) Uani 1 1 d D . . . .
C22 C 0.1968(4) 0.2137(3) 0.5141(3) 0.0443(8) Uani 1 1 d D . . . .
H22A H 0.124714 0.156729 0.443396 0.066 Uiso 1 1 calc GR . . . .
H22B H 0.179286 0.216392 0.580992 0.066 Uiso 1 1 calc GR . . . .
H22C H 0.258485 0.184900 0.505900 0.066 Uiso 1 1 calc GR . . . .
C23 C 0.8369(3) 0.7344(4) 1.0476(4) 0.0492(8) Uani 1 1 d . . . . .
C24 C 0.2241(6) -0.0163(8) 0.1983(6) 0.0405(14) Uani 0.541(3) 1 d . . P A 1
C24B C 0.2424(7) 0.0552(9) 0.2247(7) 0.0381(16) Uani 0.459(3) 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O1 1.439(3) . ?
S1 O2 1.442(3) . ?
S1 O3 1.439(3) . ?
S1 C23 1.817(4) . ?
S2 O4 1.440(4) . ?
S2 O5 1.440(2) . ?
S2 O6 1.481(3) . ?
S2 C24 1.829(7) . ?
S2B O4B 1.438(5) . ?
S2B O5 1.437(3) . ?
S2B O6 1.465(3) . ?
S2B C24B 1.820(9) . ?
Si1 N2 1.864(3) 2_666 ?
Si1 C1 1.843(3) . ?
Si1 C2 1.846(3) . ?
Si1 C3 1.851(3) . ?
Si2 C4 1.880(3) . ?
Si2 C5 1.859(4) . ?
Si2 C6 1.866(4) . ?
Si2 C7 1.884(3) . ?
Si3 N1 1.869(3) . ?
Si3 C8 1.850(3) . ?
Si3 C9 1.844(3) . ?
Si3 C10 1.843(4) . ?
F1 C23 1.338(5) . ?
F2 C23 1.352(5) . ?
F3 C23 1.322(4) . ?
F4 C24 1.352(9) . ?
F4B C24B 1.348(10) . ?
F5 C24 1.305(7) . ?
F5 C24B 1.403(8) . ?
F6 C24 1.365(8) . ?
F6 C24B 1.324(8) . ?
N1 C11 1.350(4) . ?
N1 C15 1.342(4) . ?
N2 C16 1.351(4) . ?
N2 C20 1.350(4) . ?
N3 C21 1.132(5) . ?
N4 C25 1.125(19) . ?
C25 C26 1.481(16) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.546(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.548(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11 0.9300 . ?
C11 C12 1.370(5) . ?
C12 H12 0.9300 . ?
C12 C13 1.399(4) . ?
C13 C14 1.378(4) . ?
C13 C18 1.477(4) . ?
C14 H14 0.9300 . ?
C14 C15 1.374(4) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C16 C17 1.372(4) . ?
C17 H17 0.9300 . ?
C17 C18 1.405(4) . ?
C18 C19 1.386(4) . ?
C19 H19 0.9300 . ?
C19 C20 1.377(4) . ?
C20 H20 0.9300 . ?
C21 C22 1.464(5) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 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
O1 S1 O2 114.88(18) . . ?
O1 S1 C23 103.6(2) . . ?
O2 S1 C23 103.83(18) . . ?
O3 S1 O1 114.07(17) . . ?
O3 S1 O2 115.57(18) . . ?
O3 S1 C23 102.63(17) . . ?
O4 S2 O5 113.9(2) . . ?
O4 S2 O6 117.7(2) . . ?
O4 S2 C24 102.9(4) . . ?
O5 S2 O6 113.18(17) . . ?
O5 S2 C24 103.3(3) . . ?
O6 S2 C24 103.5(3) . . ?
O4B S2B O6 119.2(3) . . ?
O4B S2B C24B 103.4(4) . . ?
O5 S2B O4B 113.6(3) . . ?
O5 S2B O6 114.33(19) . . ?
O5 S2B C24B 104.1(3) . . ?
O6 S2B C24B 98.9(3) . . ?
C1 Si1 N2 104.57(14) . 2_666 ?
C1 Si1 C2 113.00(16) . . ?
C1 Si1 C3 116.25(15) . . ?
C2 Si1 N2 106.28(13) . 2_666 ?
C2 Si1 C3 111.97(16) . . ?
C3 Si1 N2 103.48(13) . 2_666 ?
C4 Si2 C7 107.78(14) . . ?
C5 Si2 C4 110.77(17) . . ?
C5 Si2 C6 110.4(2) . . ?
C5 Si2 C7 109.73(16) . . ?
C6 Si2 C4 109.26(17) . . ?
C6 Si2 C7 108.89(17) . . ?
C8 Si3 N1 106.15(12) . . ?
C9 Si3 N1 103.34(14) . . ?
C9 Si3 C8 112.70(15) . . ?
C10 Si3 N1 104.81(14) . . ?
C10 Si3 C8 114.08(16) . . ?
C10 Si3 C9 114.42(17) . . ?
C11 N1 Si3 119.1(2) . . ?
C15 N1 Si3 122.5(2) . . ?
C15 N1 C11 118.3(3) . . ?
C16 N2 Si1 120.84(19) . 2_666 ?
C20 N2 Si1 119.9(2) . 2_666 ?
C20 N2 C16 119.2(3) . . ?
N4 C25 C26 177(4) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
Si1 C1 H1A 109.5 . . ?
Si1 C1 H1B 109.5 . . ?
Si1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si1 C3 H3A 109.0 . . ?
Si1 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
C4 C3 Si1 112.8(2) . . ?
C4 C3 H3A 109.0 . . ?
C4 C3 H3B 109.0 . . ?
Si2 C4 H4A 108.8 . . ?
Si2 C4 H4B 108.8 . . ?
C3 C4 Si2 113.6(2) . . ?
C3 C4 H4A 108.8 . . ?
C3 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
Si2 C5 H5A 109.5 . . ?
Si2 C5 H5B 109.5 . . ?
Si2 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
Si2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si2 C7 H7A 109.2 . . ?
Si2 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
C8 C7 Si2 112.2(2) . . ?
C8 C7 H7A 109.2 . . ?
C8 C7 H7B 109.2 . . ?
Si3 C8 H8A 107.8 . . ?
Si3 C8 H8B 107.8 . . ?
C7 C8 Si3 118.0(2) . . ?
C7 C8 H8A 107.8 . . ?
C7 C8 H8B 107.8 . . ?
H8A C8 H8B 107.1 . . ?
Si3 C9 H9A 109.5 . . ?
Si3 C9 H9B 109.5 . . ?
Si3 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si3 C10 H10A 109.5 . . ?
Si3 C10 H10B 109.5 . . ?
Si3 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 H11 118.9 . . ?
N1 C11 C12 122.1(3) . . ?
C12 C11 H11 118.9 . . ?
C11 C12 H12 120.3 . . ?
C11 C12 C13 119.4(3) . . ?
C13 C12 H12 120.3 . . ?
C12 C13 C18 119.7(3) . . ?
C14 C13 C12 118.1(3) . . ?
C14 C13 C18 122.2(3) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 C13 119.6(3) . . ?
C15 C14 H14 120.2 . . ?
N1 C15 C14 122.5(3) . . ?
N1 C15 H15 118.7 . . ?
C14 C15 H15 118.7 . . ?
N2 C16 H16 118.9 . . ?
N2 C16 C17 122.1(3) . . ?
C17 C16 H16 118.9 . . ?
C16 C17 H17 120.4 . . ?
C16 C17 C18 119.1(3) . . ?
C18 C17 H17 120.4 . . ?
C17 C18 C13 121.6(3) . . ?
C19 C18 C13 120.5(3) . . ?
C19 C18 C17 117.9(3) . . ?
C18 C19 H19 119.8 . . ?
C20 C19 C18 120.3(3) . . ?
C20 C19 H19 119.8 . . ?
N2 C20 C19 121.2(3) . . ?
N2 C20 H20 119.4 . . ?
C19 C20 H20 119.4 . . ?
N3 C21 C22 179.0(5) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
F1 C23 S1 111.3(3) . . ?
F1 C23 F2 107.2(3) . . ?
F2 C23 S1 110.2(3) . . ?
F3 C23 S1 113.4(3) . . ?
F3 C23 F1 107.6(3) . . ?
F3 C23 F2 106.9(3) . . ?
F4 C24 S2 109.9(5) . . ?
F4 C24 F6 111.2(6) . . ?
F5 C24 S2 109.2(5) . . ?
F5 C24 F4 111.4(6) . . ?
F5 C24 F6 107.0(5) . . ?
F6 C24 S2 108.1(5) . . ?
F4B C24B S2B 109.6(6) . . ?
F4B C24B F5 110.4(6) . . ?
F5 C24B S2B 108.3(5) . . ?
F6 C24B S2B 111.8(5) . . ?
F6 C24B F4B 112.6(7) . . ?
F6 C24B F5 103.9(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Si1 N2 C16 C17 -178.7(2) 2_666 . . . ?
Si1 N2 C20 C19 178.1(2) 2_666 . . . ?
Si1 C3 C4 Si2 172.54(16) . . . . ?
Si2 C7 C8 Si3 174.60(16) . . . . ?
Si3 N1 C11 C12 -176.7(3) . . . . ?
Si3 N1 C15 C14 176.6(2) . . . . ?
O1 S1 C23 F1 179.5(3) . . . . ?
O1 S1 C23 F2 60.7(3) . . . . ?
O1 S1 C23 F3 -59.0(3) . . . . ?
O2 S1 C23 F1 -60.2(3) . . . . ?
O2 S1 C23 F2 -179.0(3) . . . . ?
O2 S1 C23 F3 61.3(3) . . . . ?
O3 S1 C23 F1 60.5(3) . . . . ?
O3 S1 C23 F2 -58.3(3) . . . . ?
O3 S1 C23 F3 -178.0(3) . . . . ?
O4 S2 C24 F4 -175.0(4) . . . . ?
O4 S2 C24 F5 -52.6(6) . . . . ?
O4 S2 C24 F6 63.5(5) . . . . ?
O4B S2B C24B F4B 177.5(5) . . . . ?
O4B S2B C24B F5 56.9(6) . . . . ?
O4B S2B C24B F6 -57.0(6) . . . . ?
O5 S2 C24 F4 -56.3(5) . . . . ?
O5 S2 C24 F5 66.2(5) . . . . ?
O5 S2 C24 F6 -177.7(4) . . . . ?
O5 S2B C24B F4B 58.5(5) . . . . ?
O5 S2B C24B F5 -62.0(5) . . . . ?
O5 S2B C24B F6 -175.9(5) . . . . ?
O6 S2 C24 F4 61.9(5) . . . . ?
O6 S2 C24 F5 -175.6(4) . . . . ?
O6 S2 C24 F6 -59.5(5) . . . . ?
O6 S2B C24B F4B -59.5(5) . . . . ?
O6 S2B C24B F5 180.0(5) . . . . ?
O6 S2B C24B F6 66.1(6) . . . . ?
N1 Si3 C8 C7 63.0(3) . . . . ?
N1 C11 C12 C13 0.1(6) . . . . ?
N2 Si1 C3 C4 -175.3(2) 2_666 . . . ?
N2 C16 C17 C18 0.1(5) . . . . ?
C1 Si1 C3 C4 70.7(3) . . . . ?
C2 Si1 C3 C4 -61.2(3) . . . . ?
C4 Si2 C7 C8 51.6(2) . . . . ?
C5 Si2 C4 C3 170.9(2) . . . . ?
C5 Si2 C7 C8 -69.1(3) . . . . ?
C6 Si2 C4 C3 -67.3(3) . . . . ?
C6 Si2 C7 C8 170.0(2) . . . . ?
C7 Si2 C4 C3 50.9(3) . . . . ?
C8 Si3 N1 C11 -167.5(3) . . . . ?
C8 Si3 N1 C15 16.2(3) . . . . ?
C9 Si3 N1 C11 73.7(3) . . . . ?
C9 Si3 N1 C15 -102.6(3) . . . . ?
C9 Si3 C8 C7 175.4(2) . . . . ?
C10 Si3 N1 C11 -46.5(3) . . . . ?
C10 Si3 N1 C15 137.3(3) . . . . ?
C10 Si3 C8 C7 -51.9(3) . . . . ?
C11 N1 C15 C14 0.3(5) . . . . ?
C11 C12 C13 C14 0.0(5) . . . . ?
C11 C12 C13 C18 179.0(3) . . . . ?
C12 C13 C14 C15 0.0(5) . . . . ?
C12 C13 C18 C17 147.3(3) . . . . ?
C12 C13 C18 C19 -32.7(5) . . . . ?
C13 C14 C15 N1 -0.2(5) . . . . ?
C13 C18 C19 C20 177.4(3) . . . . ?
C14 C13 C18 C17 -33.8(5) . . . . ?
C14 C13 C18 C19 146.3(3) . . . . ?
C15 N1 C11 C12 -0.2(6) . . . . ?
C16 N2 C20 C19 0.9(5) . . . . ?
C16 C17 C18 C13 -178.1(3) . . . . ?
C16 C17 C18 C19 1.9(5) . . . . ?
C17 C18 C19 C20 -2.5(5) . . . . ?
C18 C13 C14 C15 -178.9(3) . . . . ?
C18 C19 C20 N2 1.2(5) . . . . ?
C20 N2 C16 C17 -1.6(5) . . . . ?

_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 4.882
_oxdiff_exptl_absorpt_empirical_full_min 0.434
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.627(3) 9902 18057 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.373(3) 0 18057 nmt 0.9916 -0.0276 0.0179 0.0494 1.0213 0.0151 -0.0450
-0.0160 0.9855

_twin_special_details            
;
Component 2 rotated by 2.6745° 
around [-0.44 0.52 0.74] (reciprocal) or [0.07 0.68 0.73] (direct)
;
