#------------------------------------------------------------------------------
#$Date: 2022-04-15 01:58:10 +0300 (Fri, 15 Apr 2022) $
#$Revision: 274536 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/00/7710044.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7710044
loop_
_publ_author_name
'Schäfer, Fabian'
'Mix, Andreas'
'Cati, Ninive'
'Lamm, Jan-Hendrik'
'Neumann, Beate'
'Stammler, Georg'
'Mitzel, Norbert Werner'
_publ_section_title
;
 Host guest chemistry of a bidentate silyl-triflate bis-Lewis-acid --
 complex complexation behaviour unravelled by diffusion NMR spectroscopy
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00583B
_journal_year                    2022
_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
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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)
;
_audit_update_record
;
2021-04-30 deposited with the CCDC.	2022-04-14 downloaded from the CCDC.
;
_cell_angle_alpha                115.737(4)
_cell_angle_beta                 101.219(4)
_cell_angle_gamma                107.630(4)
_cell_formula_units_Z            1
_cell_length_a                   12.5131(7)
_cell_length_b                   13.0673(6)
_cell_length_c                   13.5178(6)
_cell_measurement_reflns_used    10762
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.3500
_cell_measurement_theta_min      3.8440
_cell_volume                     1755.3(2)
_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)'
_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_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_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_number            27959
_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_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_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_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_description       irregular
_exptl_crystal_F_000             778
_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.053
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.081
_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_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0590
_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
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7365
_reflns_number_total             10019
_reflns_threshold_expression     'I > 2σ(I)'
_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)
;
_cod_data_source_file            d2dt00583b2.cif
_cod_data_source_block           compound_2_Bipy
_cod_original_cell_volume        1755.33(16)
_cod_database_code               7710044
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C48H66F10N6O12S4Si6
_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.
;
_diffrn_oxdiff_digest_frames
;
011194f140eafd0171889f1edab3dcef0d000288ac0
;
_diffrn_oxdiff_digest_hkl
;
01b04f589c3e2bd21d5a1958e11f19f7f962f2
;
_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)
;
_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_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
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'
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
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_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_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) . . . . ?
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
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
