#------------------------------------------------------------------------------
#$Date: 2025-11-29 18:59:44 +0100 (Sat 29 de Nov de 2025) $
#$Revision: 303589 $
#$URL: svn://www.crystallography.net/cod/cif/7/13/49/7134969.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_7134969
loop_
_publ_author_name
'Szathmári, Balázs'
'Holczbauer, Tamás'
'Balterer, Bence'
'Domján, Attila'
'Volk, Balázs'
'Kovács, Ilona'
'Kelemen, Zsolt'
_publ_section_title
;
 Synthesis and characterization of the first neutral hexacoordinated
 silole complexes.
;
_journal_issue                   82
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              16042
_journal_page_last               16045
_journal_paper_doi               10.1039/d5cc04234h
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C Cl3 D, C38 H34 O4 Si'
_chemical_formula_sum            'C39 H34 Cl3 D O4 Si'
_chemical_formula_weight         703.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-07-15
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7308)
;
_audit_update_record
;
2025-07-15 deposited with the CCDC.	2025-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.6550(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.05580(10)
_cell_length_b                   13.59260(10)
_cell_length_c                   23.50010(10)
_cell_measurement_reflns_used    58852
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.9090
_cell_measurement_theta_min      3.2620
_cell_volume                     3445.73(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.143a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 42.58a 64-bit (release 31-05-2022))'
_computing_data_reduction        'CrysAlisPro 1.171.43.143a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -122.00 -29.00   0.50    0.05    --  -47.20  -9.00-152.00  186
  2  ω     25.00 120.00   0.50    0.05    --   47.20  77.00-180.00  190
  3  ω     25.00 120.00   0.50    0.05    --   47.20  77.00  30.00  190
  4  ω     25.00 120.00   0.50    0.05    --   47.20  77.00  60.00  190
  5  ω     25.00 120.00   0.50    0.05    --   47.20  77.00 -30.00  190
  6  ω     25.00 120.00   0.50    0.05    --   47.20  77.00-120.00  190
  7  ω     25.00  87.00   0.50    0.05    --   47.20  77.00 -90.00  124
  8  ω     29.00 122.00   0.50    0.05    --   47.20   9.00  21.00  186
  9  ω    -22.00  28.00   0.50    0.05    --  -47.20   9.00  21.00  100
 10  ω   -112.00 -26.00   0.50    0.05    --  -99.00 125.00  30.00  172
 11  ω     32.00 120.00   0.50    0.05    --   47.20  57.00 150.00  176
 12  ω     87.00 178.00   0.50    0.05    --  105.24   9.00  21.00  182
 13  ω     92.00 178.00   0.50    0.05    --  105.24  15.00 -30.00  172
 14  ω    -27.00  30.00   0.50    0.05    --   47.20 -19.00-120.00  114
 15  ω    -26.00  28.00   0.50    0.05    --   47.20  -9.00-152.00  108
 16  ω     33.00  75.00   0.50    0.05    --  105.24 -61.00-150.00   84
 17  ω     33.00  75.00   0.50    0.05    --  105.24 -61.00 -30.00   84
 18  ω     33.00  75.00   0.50    0.05    --  105.24 -61.00   0.00   84
 19  ω     33.00  75.00   0.50    0.05    --  105.24 -61.00  30.00   84
 20  ω     33.00  75.00   0.50    0.05    --  105.24 -61.00  60.00   84
 21  ω     19.00  95.00   0.50    0.05    --   47.20-125.00 120.00  152
 22  ω     33.00 112.00   0.50    0.05    --  105.24-125.00 150.00  158
 23  ω     33.00 105.00   0.50    0.05    --  105.24 -95.00 150.00  144
 24  ω     33.00 105.00   0.50    0.05    --  105.24 -95.00  60.00  144
 25  ω     33.00 105.00   0.50    0.05    --  105.24 -95.00 -60.00  144
 26  ω     33.00 105.00   0.50    0.05    --  105.24 -95.00-120.00  144
 27  ω     33.00 105.00   0.50    0.05    --  105.24 -95.00-180.00  144
 28  ω     19.00  95.00   0.50    0.05    --   47.20-125.00 -60.00  152
 29  ω   -172.00 -76.00   0.50    0.05    --  -99.00 -77.00-180.00  192
 30  ω   -172.00 -76.00   0.50    0.05    --  -99.00 -77.00 -90.00  192
 31  ω   -172.00 -76.00   0.50    0.05    --  -99.00 -77.00  60.00  192
 32  ω   -172.00 -76.00   0.50    0.05    --  -99.00 -77.00 150.00  192
 33  ω   -172.00 -76.00   0.50    0.05    --  -99.00 -77.00  90.00  192
 34  ω   -172.00 -76.00   0.50    0.05    --  -99.00 -77.00  30.00  192
 35  ω   -172.00 -82.00   0.50    0.05    --  -99.00 -61.00  90.00  180
 36  ω   -172.00 -82.00   0.50    0.05    --  -99.00 -61.00 120.00  180
 37  ω   -172.00 -76.00   0.50    0.05    --  -99.00 -77.00   0.00  192
 38  ω   -174.00 -85.00   0.50    0.05    --  -99.00 -15.00 -60.00  178
 39  ω   -172.00 -76.00   0.50    0.05    --  -99.00 -77.00-150.00  192
 40  ω   -172.00 -76.00   0.50    0.05    --  -99.00 -77.00-120.00  192
 41  ω   -174.00 -81.00   0.50    0.05    --  -99.00  -9.00-152.00  186
 42  ω   -172.00 -82.00   0.50    0.05    --  -99.00 -61.00 -60.00  180
 43  ω   -174.00 -85.00   0.50    0.05    --  -99.00 -15.00 120.00  178
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1071931000
_diffrn_orient_matrix_UB_12      -0.0055364000
_diffrn_orient_matrix_UB_13      -0.0542583000
_diffrn_orient_matrix_UB_21      -0.0942555000
_diffrn_orient_matrix_UB_22      0.0121366000
_diffrn_orient_matrix_UB_23      0.0390331000
_diffrn_orient_matrix_UB_31      0.0049789000
_diffrn_orient_matrix_UB_32      0.1125450000
_diffrn_orient_matrix_UB_33      -0.0068184000
_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  0.0410
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            81206
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.440
_diffrn_reflns_theta_min         1.927
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.069
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.366
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.143a (Rigaku Oxford Diffraction, 2024)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.354
_exptl_crystal_size_mid          0.329
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
 Flack x determined using 6320 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     894
_refine_ls_number_reflns         13750
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0405
_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)+(0.0808P)²+0.7716P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1117
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.925
_reflns_number_gt                13357
_reflns_number_total             13750
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5cc04234h3.cif
_cod_data_source_block           sb225kr2_auto
_cod_depositor_comments
'Adding full bibliography for 7134962--7134969.cif.'
_cod_database_code               7134969
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C38H34O4Si1
_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.
;
_cell_oxdiff_angle_alpha         90.0440(9)
_cell_oxdiff_angle_beta          102.6596(9)
_cell_oxdiff_angle_gamma         90.0244(9)
_cell_oxdiff_length_a            11.05505(12)
_cell_oxdiff_length_b            13.59327(16)
_cell_oxdiff_length_c            23.5009(2)
_cell_oxdiff_measurement_reflns_used 58852
_cell_oxdiff_volume              3445.73(7)
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.609(11)
 0.391(11)
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
 Cl5A-C78 \\sim Cl5B-C78
 with sigma of 0.02
 Cl4A-C78 \\sim Cl4B-C78
 with sigma of 0.02
 Cl3A-C77 \\sim Cl3B-C77
 with sigma of 0.02
 Cl1A-C77 \\sim Cl1B-C77
 with sigma of 0.02
4. Others
 Sof(D78A)=Sof(Cl4B)=Sof(Cl5B)=1-FVAR(1)
 Sof(D78)=Sof(Cl4A)=Sof(Cl5A)=FVAR(1)
 Sof(D77A)=Sof(Cl1B)=Sof(Cl3B)=1-FVAR(2)
 Sof(D77)=Sof(Cl1A)=Sof(Cl3A)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C77(D77), C77(D77A), C78(D78), C78(D78A)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C11(H11), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22),
 C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31),
  C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C44(H44),
 C50(H50), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C60(H60), C61(H61),
  C62(H62), C63(H63), C64(H64), C66(H66), C67(H67), C68(H68), C69(H69),
 C70(H70), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C52(H52A,H52B,
 H52C)
;
_ins_header
;
TITL SB225Kr2_auto in Pn 
REM Pn (#7 in standard setting)
CELL 1.54184  11.055795  13.592558  23.500131  90.0000 102.6548  90.0000
ZERR    5.00   0.000055   0.000077   0.000123   0.0000   0.0005   0.0000
LATT -1
SYMM  x+1/2,-y, z+1/2 
SFAC C H O Si
UNIT 190.00 170.00 20.00 5.00
REM  CrysAlisPro recorded range (K): Min=99.9; max=100.1; aver:100.0
TEMP -173
SIZE 0.20 0.33 0.35
TREF
HKLF 4
END
;
_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 1.868
_oxdiff_exptl_absorpt_empirical_full_min 0.566
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y, z+1/2'
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
Cl2 Cl 0.51286(10) 0.79363(9) 0.33140(5) 0.0531(3) Uani 1 1 d . . . . .
C77 C 0.4696(4) 0.9145(4) 0.30499(19) 0.0530(12) Uani 1 1 d D . . . .
D77 D 0.508433 0.962790 0.335695 0.064 Uiso 0.63(2) 1 calc R U P A 1
D77A D 0.491056 0.963559 0.337341 0.064 Uiso 0.37(2) 1 calc R U P A 2
Cl1A Cl 0.3113(5) 0.9299(5) 0.2912(3) 0.0839(19) Uani 0.63(2) 1 d D . P A 1
Cl3A Cl 0.5250(4) 0.9397(3) 0.24046(19) 0.0441(10) Uani 0.63(2) 1 d D . P A 1
Cl1B Cl 0.2971(9) 0.9020(15) 0.2805(4) 0.105(4) Uani 0.37(2) 1 d D . P A 2
Cl3B Cl 0.5337(11) 0.9436(8) 0.2528(9) 0.102(4) Uani 0.37(2) 1 d D . P A 2
Cl5 Cl 0.49862(9) 0.71460(7) 0.66490(4) 0.0402(2) Uani 1 1 d . . . . .
C78 C 0.5957(4) 0.6117(3) 0.68273(19) 0.0475(10) Uani 1 1 d D . . . .
D78 D 0.613960 0.586233 0.645568 0.057 Uiso 0.595(16) 1 calc R U P B 1
D78A D 0.604494 0.574861 0.647007 0.057 Uiso 0.405(16) 1 calc R U P B 2
Cl4A Cl 0.5311(3) 0.5172(3) 0.71379(15) 0.0494(10) Uani 0.595(16) 1 d D . P B 1
Cl5A Cl 0.7404(3) 0.6480(3) 0.72865(16) 0.0329(8) Uani 0.595(16) 1 d D . P B 1
Cl4B Cl 0.4960(14) 0.5378(9) 0.7276(8) 0.143(6) Uani 0.405(16) 1 d D . P B 2
Cl5B Cl 0.7271(8) 0.6277(11) 0.7264(3) 0.092(3) Uani 0.405(16) 1 d D . P B 2
Si1 Si 0.71969(7) 0.49340(6) 0.39109(3) 0.01632(17) Uani 1 1 d . . . . .
O1 O 0.88695(19) 0.47880(16) 0.39420(10) 0.0204(4) Uani 1 1 d . . . . .
O2 O 0.73658(19) 0.62804(15) 0.39428(9) 0.0195(4) Uani 1 1 d . . . . .
O3 O 0.7103(2) 0.50924(16) 0.31264(9) 0.0199(4) Uani 1 1 d . . . . .
O4 O 0.5546(2) 0.51714(16) 0.38228(10) 0.0210(4) Uani 1 1 d . . . . .
C1 C 0.7416(3) 0.4787(2) 0.47466(13) 0.0173(6) Uani 1 1 d . . . . .
C2 C 0.7456(3) 0.3827(2) 0.48933(12) 0.0187(6) Uani 1 1 d . . . . .
C3 C 0.7163(3) 0.3112(2) 0.43922(13) 0.0182(6) Uani 1 1 d . . . . .
C4 C 0.6987(3) 0.3528(2) 0.38558(13) 0.0175(6) Uani 1 1 d . . . . .
C5 C 0.9738(3) 0.5391(2) 0.41617(13) 0.0211(6) Uani 1 1 d . . . . .
C6 C 0.9534(3) 0.6355(2) 0.43042(14) 0.0235(6) Uani 1 1 d . . . . .
H6 H 1.021130 0.674165 0.450385 0.028 Uiso 1 1 calc R U . . .
C7 C 0.8363(3) 0.6768(2) 0.41616(12) 0.0199(6) Uani 1 1 d . . . . .
C8 C 1.1027(3) 0.4988(3) 0.42483(19) 0.0330(8) Uani 1 1 d . . . . .
H8A H 1.117857 0.452830 0.457774 0.049 Uiso 1 1 calc R U . . .
H8B H 1.162552 0.552891 0.432936 0.049 Uiso 1 1 calc R U . . .
H8C H 1.111966 0.464183 0.389439 0.049 Uiso 1 1 calc R U . . .
C9 C 0.8179(3) 0.7849(2) 0.42413(16) 0.0288(7) Uani 1 1 d . . . . .
H9A H 0.787555 0.815768 0.385975 0.043 Uiso 1 1 calc R U . . .
H9B H 0.897036 0.814952 0.443212 0.043 Uiso 1 1 calc R U . . .
H9C H 0.757266 0.794668 0.448391 0.043 Uiso 1 1 calc R U . . .
C10 C 0.6147(3) 0.5198(2) 0.27132(14) 0.0207(6) Uani 1 1 d . . . . .
C11 C 0.4951(3) 0.5291(3) 0.27983(14) 0.0268(7) Uani 1 1 d . . . . .
H11 H 0.428155 0.536679 0.247014 0.032 Uiso 1 1 calc R U . . .
C12 C 0.4711(3) 0.5277(2) 0.33563(14) 0.0225(6) Uani 1 1 d . . . . .
C13 C 0.6388(3) 0.5205(3) 0.21086(14) 0.0273(7) Uani 1 1 d . . . . .
H13A H 0.714292 0.558277 0.210776 0.041 Uiso 1 1 calc R U . . .
H13B H 0.568485 0.550911 0.183928 0.041 Uiso 1 1 calc R U . . .
H13C H 0.649452 0.452834 0.198441 0.041 Uiso 1 1 calc R U . . .
C14 C 0.3420(3) 0.5385(3) 0.34466(18) 0.0367(9) Uani 1 1 d . . . . .
H14A H 0.312867 0.474889 0.356097 0.055 Uiso 1 1 calc R U . . .
H14B H 0.287207 0.560683 0.308328 0.055 Uiso 1 1 calc R U . . .
H14C H 0.341256 0.586892 0.375479 0.055 Uiso 1 1 calc R U . . .
C15 C 0.7598(3) 0.5597(2) 0.51767(13) 0.0191(6) Uani 1 1 d . . . . .
C16 C 0.6695(3) 0.6323(2) 0.51353(14) 0.0228(6) Uani 1 1 d . . . . .
H16 H 0.596923 0.628314 0.483247 0.027 Uiso 1 1 calc R U . . .
C17 C 0.6827(3) 0.7109(2) 0.55271(15) 0.0281(7) Uani 1 1 d . . . . .
H17 H 0.619692 0.759484 0.549075 0.034 Uiso 1 1 calc R U . . .
C18 C 0.7888(3) 0.7176(3) 0.59710(15) 0.0297(7) Uani 1 1 d . . . . .
H18 H 0.798304 0.770650 0.624011 0.036 Uiso 1 1 calc R U . . .
C19 C 0.8802(3) 0.6469(2) 0.60198(15) 0.0265(7) Uani 1 1 d . . . . .
H19 H 0.952766 0.651766 0.632184 0.032 Uiso 1 1 calc R U . . .
C20 C 0.8668(3) 0.5684(2) 0.56295(14) 0.0219(6) Uani 1 1 d . . . . .
H20 H 0.930341 0.520282 0.566842 0.026 Uiso 1 1 calc R U . . .
C21 C 0.7826(3) 0.3461(2) 0.55040(13) 0.0197(6) Uani 1 1 d . . . . .
C22 C 0.7192(3) 0.3749(2) 0.59324(13) 0.0236(6) Uani 1 1 d . . . . .
H22 H 0.647724 0.415401 0.582999 0.028 Uiso 1 1 calc R U . . .
C23 C 0.7608(4) 0.3441(3) 0.65091(15) 0.0328(8) Uani 1 1 d . . . . .
H23 H 0.717804 0.364170 0.679772 0.039 Uiso 1 1 calc R U . . .
C24 C 0.8637(4) 0.2848(3) 0.66621(15) 0.0373(9) Uani 1 1 d . . . . .
H24 H 0.891575 0.264382 0.705564 0.045 Uiso 1 1 calc R U . . .
C25 C 0.9269(4) 0.2548(3) 0.62411(16) 0.0339(8) Uani 1 1 d . . . . .
H25 H 0.997712 0.213504 0.634511 0.041 Uiso 1 1 calc R U . . .
C26 C 0.8855(3) 0.2858(2) 0.56638(15) 0.0259(7) Uani 1 1 d . . . . .
H26 H 0.928576 0.265226 0.537652 0.031 Uiso 1 1 calc R U . . .
C27 C 0.6963(3) 0.2049(2) 0.44896(13) 0.0186(6) Uani 1 1 d . . . . .
C28 C 0.6224(3) 0.1736(2) 0.48712(13) 0.0204(6) Uani 1 1 d . . . . .
H28 H 0.594045 0.220673 0.511095 0.024 Uiso 1 1 calc R U . . .
C29 C 0.5900(3) 0.0760(3) 0.49060(15) 0.0246(7) Uani 1 1 d . . . . .
H29 H 0.538175 0.057042 0.516029 0.029 Uiso 1 1 calc R U . . .
C30 C 0.6330(3) 0.0056(2) 0.45703(15) 0.0257(7) Uani 1 1 d . . . . .
H30 H 0.608615 -0.061212 0.458366 0.031 Uiso 1 1 calc R U . . .
C31 C 0.7127(3) 0.0343(3) 0.42115(15) 0.0276(7) Uani 1 1 d . . . . .
H31 H 0.745883 -0.013750 0.399442 0.033 Uiso 1 1 calc R U . . .
C32 C 0.7432(3) 0.1323(2) 0.41732(14) 0.0233(6) Uani 1 1 d . . . . .
H32 H 0.797000 0.150783 0.392714 0.028 Uiso 1 1 calc R U . . .
C33 C 0.6543(3) 0.2978(2) 0.33034(13) 0.0189(6) Uani 1 1 d . . . . .
C34 C 0.5391(3) 0.2514(2) 0.31870(14) 0.0244(6) Uani 1 1 d . . . . .
H34 H 0.489047 0.254100 0.346752 0.029 Uiso 1 1 calc R U . . .
C35 C 0.4963(4) 0.2011(3) 0.26639(15) 0.0318(8) Uani 1 1 d . . . . .
H35 H 0.417103 0.170657 0.258918 0.038 Uiso 1 1 calc R U . . .
C36 C 0.5687(4) 0.1955(3) 0.22539(15) 0.0333(8) Uani 1 1 d . . . . .
H36 H 0.539980 0.160368 0.190056 0.040 Uiso 1 1 calc R U . . .
C37 C 0.6833(3) 0.2414(2) 0.23627(14) 0.0271(7) Uani 1 1 d . . . . .
H37 H 0.733463 0.237410 0.208292 0.033 Uiso 1 1 calc R U . . .
C38 C 0.7256(3) 0.2934(2) 0.28784(14) 0.0232(6) Uani 1 1 d . . . . .
H38 H 0.803343 0.326040 0.294301 0.028 Uiso 1 1 calc R U . . .
Si2 Si 0.28020(7) 0.01331(6) 0.60849(3) 0.01591(17) Uani 1 1 d . . . . .
O5 O 0.11292(19) 0.02644(16) 0.60608(9) 0.0201(4) Uani 1 1 d . . . . .
O6 O 0.26491(19) -0.12150(15) 0.60536(9) 0.0194(4) Uani 1 1 d . . . . .
O7 O 0.29135(19) -0.00202(16) 0.68711(9) 0.0197(4) Uani 1 1 d . . . . .
O8 O 0.44583(19) -0.00898(16) 0.61681(9) 0.0204(4) Uani 1 1 d . . . . .
C39 C 0.2558(3) 0.0281(2) 0.52484(13) 0.0180(6) Uani 1 1 d . . . . .
C40 C 0.2487(3) 0.1247(2) 0.51071(13) 0.0167(5) Uani 1 1 d . . . . .
C41 C 0.2813(3) 0.1954(2) 0.56086(12) 0.0182(6) Uani 1 1 d . . . . .
C42 C 0.3006(3) 0.1538(2) 0.61424(12) 0.0174(6) Uani 1 1 d . . . . .
C43 C 0.0264(3) -0.0335(2) 0.58258(13) 0.0202(6) Uani 1 1 d . . . . .
C44 C 0.0492(3) -0.1302(2) 0.56827(13) 0.0227(6) Uani 1 1 d . . . . .
H44 H -0.017911 -0.169482 0.548346 0.027 Uiso 1 1 calc R U . . .
C45 C 0.1675(3) -0.1710(2) 0.58234(13) 0.0203(6) Uani 1 1 d . . . . .
C46 C -0.1018(3) 0.0057(3) 0.57268(17) 0.0307(8) Uani 1 1 d . . . . .
H46A H -0.116671 0.032410 0.609273 0.046 Uiso 1 1 calc R U . . .
H46B H -0.161014 -0.047405 0.558965 0.046 Uiso 1 1 calc R U . . .
H46C H -0.112443 0.057920 0.543256 0.046 Uiso 1 1 calc R U . . .
C47 C 0.1871(3) -0.2773(2) 0.57263(15) 0.0269(7) Uani 1 1 d . . . . .
H47A H 0.229120 -0.285079 0.540254 0.040 Uiso 1 1 calc R U . . .
H47B H 0.106807 -0.310960 0.563160 0.040 Uiso 1 1 calc R U . . .
H47C H 0.238345 -0.306045 0.608082 0.040 Uiso 1 1 calc R U . . .
C48 C 0.3629(3) -0.0216(3) 0.78845(14) 0.0256(7) Uani 1 1 d . . . . .
H48A H 0.338751 0.044288 0.798801 0.038 Uiso 1 1 calc R U . . .
H48B H 0.438515 -0.041994 0.816135 0.038 Uiso 1 1 calc R U . . .
H48C H 0.296092 -0.068205 0.789898 0.038 Uiso 1 1 calc R U . . .
C49 C 0.3865(3) -0.0197(2) 0.72817(13) 0.0195(6) Uani 1 1 d . . . . .
C50 C 0.5045(3) -0.0349(3) 0.71816(14) 0.0252(7) Uani 1 1 d . . . . .
H50 H 0.570180 -0.050985 0.750177 0.030 Uiso 1 1 calc R U . . .
C51 C 0.5292(3) -0.0273(2) 0.66331(14) 0.0213(6) Uani 1 1 d . . . . .
C52 C 0.6566(3) -0.0395(3) 0.65277(16) 0.0321(8) Uani 1 1 d . . . . .
H52A H 0.652892 -0.079664 0.617778 0.048 Uiso 1 1 calc R U . . .
H52B H 0.709416 -0.072193 0.686418 0.048 Uiso 1 1 calc R U . . .
H52C H 0.691312 0.025193 0.647195 0.048 Uiso 1 1 calc R U . . .
C53 C 0.2382(3) -0.0519(2) 0.48087(13) 0.0188(6) Uani 1 1 d . . . . .
C54 C 0.3321(3) -0.1228(2) 0.48456(14) 0.0230(6) Uani 1 1 d . . . . .
H54 H 0.404317 -0.118723 0.515027 0.028 Uiso 1 1 calc R U . . .
C55 C 0.3208(3) -0.1989(3) 0.44423(15) 0.0271(7) Uani 1 1 d . . . . .
H55 H 0.385345 -0.245960 0.447147 0.033 Uiso 1 1 calc R U . . .
C56 C 0.2156(3) -0.2064(3) 0.39973(15) 0.0288(7) Uani 1 1 d . . . . .
H56 H 0.207973 -0.258351 0.372156 0.035 Uiso 1 1 calc R U . . .
C57 C 0.1214(3) -0.1372(2) 0.39577(14) 0.0253(7) Uani 1 1 d . . . . .
H57 H 0.049057 -0.141943 0.365421 0.030 Uiso 1 1 calc R U . . .
C58 C 0.1328(3) -0.0613(2) 0.43604(14) 0.0213(6) Uani 1 1 d . . . . .
H58 H 0.067615 -0.014789 0.433035 0.026 Uiso 1 1 calc R U . . .
C59 C 0.2040(3) 0.1631(2) 0.45023(12) 0.0180(6) Uani 1 1 d . . . . .
C60 C 0.0960(3) 0.2202(2) 0.43839(14) 0.0240(6) Uani 1 1 d . . . . .
H60 H 0.057263 0.236681 0.469431 0.029 Uiso 1 1 calc R U . . .
C61 C 0.0443(3) 0.2532(3) 0.38286(16) 0.0296(7) Uani 1 1 d . . . . .
H61 H -0.029975 0.290707 0.375819 0.036 Uiso 1 1 calc R U . . .
C62 C 0.1013(3) 0.2314(3) 0.33742(15) 0.0324(8) Uani 1 1 d . . . . .
H62 H 0.066595 0.254016 0.299074 0.039 Uiso 1 1 calc R U . . .
C63 C 0.2094(3) 0.1761(3) 0.34844(14) 0.0301(7) Uani 1 1 d . . . . .
H63 H 0.248917 0.161396 0.317379 0.036 Uiso 1 1 calc R U . . .
C64 C 0.2611(3) 0.1416(2) 0.40445(14) 0.0241(6) Uani 1 1 d . . . . .
H64 H 0.335024 0.103701 0.411311 0.029 Uiso 1 1 calc R U . . .
C65 C 0.3024(3) 0.3020(2) 0.55096(12) 0.0193(6) Uani 1 1 d . . . . .
C66 C 0.3722(3) 0.3323(2) 0.51103(13) 0.0208(6) Uani 1 1 d . . . . .
H66 H 0.397480 0.284929 0.486270 0.025 Uiso 1 1 calc R U . . .
C67 C 0.4053(3) 0.4302(3) 0.50690(15) 0.0247(6) Uani 1 1 d . . . . .
H67 H 0.454410 0.448832 0.480179 0.030 Uiso 1 1 calc R U . . .
C68 C 0.3665(3) 0.5012(3) 0.54201(16) 0.0284(7) Uani 1 1 d . . . . .
H68 H 0.390453 0.568018 0.540123 0.034 Uiso 1 1 calc R U . . .
C69 C 0.2927(4) 0.4725(3) 0.57956(15) 0.0301(7) Uani 1 1 d . . . . .
H69 H 0.264008 0.520557 0.602808 0.036 Uiso 1 1 calc R U . . .
C70 C 0.2598(3) 0.3745(2) 0.58390(14) 0.0255(7) Uani 1 1 d . . . . .
H70 H 0.207794 0.356721 0.609504 0.031 Uiso 1 1 calc R U . . .
C71 C 0.3511(3) 0.2054(2) 0.66978(13) 0.0187(6) Uani 1 1 d . . . . .
C72 C 0.4760(3) 0.2321(3) 0.68464(14) 0.0267(7) Uani 1 1 d . . . . .
H72 H 0.527573 0.220379 0.657894 0.032 Uiso 1 1 calc R U . . .
C73 C 0.5259(4) 0.2759(3) 0.73842(16) 0.0355(8) Uani 1 1 d . . . . .
H73 H 0.611246 0.293121 0.748145 0.043 Uiso 1 1 calc R U . . .
C74 C 0.4517(4) 0.2944(3) 0.77762(14) 0.0314(8) Uani 1 1 d . . . . .
H74 H 0.485479 0.325725 0.813755 0.038 Uiso 1 1 calc R U . . .
C75 C 0.3288(4) 0.2673(3) 0.76401(14) 0.0299(7) Uani 1 1 d . . . . .
H75 H 0.277698 0.279473 0.790909 0.036 Uiso 1 1 calc R U . . .
C76 C 0.2793(3) 0.2220(3) 0.71097(14) 0.0257(7) Uani 1 1 d . . . . .
H76 H 0.194919 0.201926 0.702542 0.031 Uiso 1 1 calc R U . . .
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'
D D 0.0000 0.0000 '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'
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
1 9 -1 0.1067
5 0 8 0.1315
-4 -6 -4 0.1040
-3 6 -7 0.1768
5 4 -11 0.1251
5 -3 -11 0.1403
-2 -8 6 0.1358
-4 6 9 0.1076
1 9 0 0.1065
-2 5 -10 0.1834
-3 -7 -7 0.1071
-1 -9 1 0.0952
2 -5 10 0.1627
3 3 11 0.1171
0 9 0 0.1001
-5 6 8 0.1088
-6 -2 11 0.1965
0 -9 1 0.1062
6 -3 -11 0.1489
5 5 -9 0.1205
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
Cl2 C77 D77 108.3 . . ?
Cl2 C77 D77A 110.4 . . ?
Cl2 C77 Cl3A 110.9(3) . . ?
Cl2 C77 Cl1B 101.6(6) . . ?
Cl1A C77 Cl2 111.2(4) . . ?
Cl1A C77 D77 108.3 . . ?
Cl1A C77 Cl3A 109.9(3) . . ?
Cl3A C77 D77 108.3 . . ?
Cl1B C77 D77A 110.4 . . ?
Cl3B C77 Cl2 111.4(5) . . ?
Cl3B C77 D77A 110.4 . . ?
Cl3B C77 Cl1B 112.3(7) . . ?
Cl5 C78 D78 107.3 . . ?
Cl5 C78 D78A 111.4 . . ?
Cl5 C78 Cl5A 110.0(3) . . ?
Cl5 C78 Cl4B 98.6(6) . . ?
Cl4A C78 Cl5 114.2(3) . . ?
Cl4A C78 D78 107.3 . . ?
Cl4A C78 Cl5A 110.6(3) . . ?
Cl5A C78 D78 107.3 . . ?
Cl4B C78 D78A 111.4 . . ?
Cl5B C78 Cl5 117.8(6) . . ?
Cl5B C78 D78A 111.4 . . ?
Cl5B C78 Cl4B 105.3(5) . . ?
O1 Si1 C1 92.71(11) . . ?
O1 Si1 C4 90.06(11) . . ?
O2 Si1 O1 90.77(10) . . ?
O2 Si1 C1 94.14(12) . . ?
O2 Si1 C4 178.33(13) . . ?
O3 Si1 O1 83.57(10) . . ?
O3 Si1 O2 84.67(10) . . ?
O3 Si1 C1 176.07(12) . . ?
O3 Si1 C4 93.98(12) . . ?
O4 Si1 O1 174.17(11) . . ?
O4 Si1 O2 85.33(10) . . ?
O4 Si1 O3 91.74(10) . . ?
O4 Si1 C1 91.89(12) . . ?
O4 Si1 C4 93.73(12) . . ?
C4 Si1 C1 87.27(13) . . ?
C5 O1 Si1 127.1(2) . . ?
C7 O2 Si1 126.6(2) . . ?
C10 O3 Si1 129.2(2) . . ?
C12 O4 Si1 129.5(2) . . ?
C2 C1 Si1 110.4(2) . . ?
C2 C1 C15 123.7(3) . . ?
C15 C1 Si1 125.8(2) . . ?
C1 C2 C3 115.8(3) . . ?
C1 C2 C21 123.8(3) . . ?
C21 C2 C3 120.3(3) . . ?
C4 C3 C2 114.9(3) . . ?
C4 C3 C27 123.5(3) . . ?
C27 C3 C2 121.3(3) . . ?
C3 C4 Si1 111.1(2) . . ?
C3 C4 C33 123.8(3) . . ?
C33 C4 Si1 124.7(2) . . ?
O1 C5 C6 123.8(3) . . ?
O1 C5 C8 115.3(3) . . ?
C6 C5 C8 120.9(3) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 C5 121.3(3) . . ?
C7 C6 H6 119.4 . . ?
O2 C7 C6 124.1(3) . . ?
O2 C7 C9 115.1(3) . . ?
C6 C7 C9 120.8(3) . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O3 C10 C11 123.9(3) . . ?
O3 C10 C13 115.5(3) . . ?
C11 C10 C13 120.6(3) . . ?
C10 C11 H11 119.4 . . ?
C10 C11 C12 121.2(3) . . ?
C12 C11 H11 119.4 . . ?
O4 C12 C11 124.0(3) . . ?
O4 C12 C14 114.9(3) . . ?
C11 C12 C14 121.1(3) . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C1 119.5(3) . . ?
C16 C15 C20 117.5(3) . . ?
C20 C15 C1 123.0(3) . . ?
C15 C16 H16 119.1 . . ?
C15 C16 C17 121.8(3) . . ?
C17 C16 H16 119.1 . . ?
C16 C17 H17 120.2 . . ?
C18 C17 C16 119.6(3) . . ?
C18 C17 H17 120.2 . . ?
C17 C18 H18 120.1 . . ?
C19 C18 C17 119.9(3) . . ?
C19 C18 H18 120.1 . . ?
C18 C19 H19 119.8 . . ?
C18 C19 C20 120.5(3) . . ?
C20 C19 H19 119.8 . . ?
C15 C20 H20 119.6 . . ?
C19 C20 C15 120.8(3) . . ?
C19 C20 H20 119.6 . . ?
C22 C21 C2 121.6(3) . . ?
C26 C21 C2 119.7(3) . . ?
C26 C21 C22 118.7(3) . . ?
C21 C22 H22 119.9 . . ?
C23 C22 C21 120.2(3) . . ?
C23 C22 H22 119.9 . . ?
C22 C23 H23 119.8 . . ?
C24 C23 C22 120.5(3) . . ?
C24 C23 H23 119.8 . . ?
C23 C24 H24 120.0 . . ?
C23 C24 C25 120.1(3) . . ?
C25 C24 H24 120.0 . . ?
C24 C25 H25 120.3 . . ?
C24 C25 C26 119.4(3) . . ?
C26 C25 H25 120.3 . . ?
C21 C26 C25 121.1(3) . . ?
C21 C26 H26 119.4 . . ?
C25 C26 H26 119.4 . . ?
C28 C27 C3 121.3(3) . . ?
C32 C27 C3 121.2(3) . . ?
C32 C27 C28 117.3(3) . . ?
C27 C28 H28 119.2 . . ?
C29 C28 C27 121.6(3) . . ?
C29 C28 H28 119.2 . . ?
C28 C29 H29 119.9 . . ?
C28 C29 C30 120.2(3) . . ?
C30 C29 H29 119.9 . . ?
C29 C30 H30 120.4 . . ?
C29 C30 C31 119.2(3) . . ?
C31 C30 H30 120.4 . . ?
C30 C31 H31 120.0 . . ?
C32 C31 C30 120.1(3) . . ?
C32 C31 H31 120.0 . . ?
C27 C32 H32 119.3 . . ?
C31 C32 C27 121.4(3) . . ?
C31 C32 H32 119.3 . . ?
C34 C33 C4 120.8(3) . . ?
C34 C33 C38 118.2(3) . . ?
C38 C33 C4 121.0(3) . . ?
C33 C34 H34 119.6 . . ?
C33 C34 C35 120.9(3) . . ?
C35 C34 H34 119.6 . . ?
C34 C35 H35 119.8 . . ?
C36 C35 C34 120.3(3) . . ?
C36 C35 H35 119.8 . . ?
C35 C36 H36 120.3 . . ?
C35 C36 C37 119.5(3) . . ?
C37 C36 H36 120.3 . . ?
C36 C37 H37 119.7 . . ?
C36 C37 C38 120.5(3) . . ?
C38 C37 H37 119.7 . . ?
C33 C38 H38 119.7 . . ?
C37 C38 C33 120.6(3) . . ?
C37 C38 H38 119.7 . . ?
O5 Si2 C39 92.47(11) . . ?
O5 Si2 C42 90.43(11) . . ?
O6 Si2 O5 90.71(10) . . ?
O6 Si2 C39 94.09(12) . . ?
O6 Si2 C42 177.99(12) . . ?
O7 Si2 O5 83.57(10) . . ?
O7 Si2 O6 84.99(10) . . ?
O7 Si2 C39 175.91(11) . . ?
O7 Si2 C42 93.50(12) . . ?
O8 Si2 O5 174.10(11) . . ?
O8 Si2 O6 85.42(10) . . ?
O8 Si2 O7 91.65(10) . . ?
O8 Si2 C39 92.25(11) . . ?
O8 Si2 C42 93.32(12) . . ?
C42 Si2 C39 87.52(13) . . ?
C43 O5 Si2 126.7(2) . . ?
C45 O6 Si2 126.8(2) . . ?
C49 O7 Si2 129.8(2) . . ?
C51 O8 Si2 129.6(2) . . ?
C40 C39 Si2 109.7(2) . . ?
C40 C39 C53 123.3(3) . . ?
C53 C39 Si2 126.9(2) . . ?
C39 C40 C41 116.0(3) . . ?
C39 C40 C59 124.2(3) . . ?
C59 C40 C41 119.7(3) . . ?
C42 C41 C40 115.0(3) . . ?
C42 C41 C65 123.6(3) . . ?
C65 C41 C40 121.2(3) . . ?
C41 C42 Si2 111.0(2) . . ?
C41 C42 C71 124.9(3) . . ?
C71 C42 Si2 123.3(2) . . ?
O5 C43 C44 123.0(3) . . ?
O5 C43 C46 115.8(3) . . ?
C44 C43 C46 121.2(3) . . ?
C43 C44 H44 119.0 . . ?
C45 C44 C43 121.9(3) . . ?
C45 C44 H44 119.0 . . ?
O6 C45 C44 123.3(3) . . ?
O6 C45 C47 115.9(3) . . ?
C44 C45 C47 120.8(3) . . ?
C43 C46 H46A 109.5 . . ?
C43 C46 H46B 109.5 . . ?
C43 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C45 C47 H47A 109.5 . . ?
C45 C47 H47B 109.5 . . ?
C45 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C49 C48 H48A 109.5 . . ?
C49 C48 H48B 109.5 . . ?
C49 C48 H48C 109.5 . . ?
O7 C49 C48 115.5(3) . . ?
O7 C49 C50 123.0(3) . . ?
C50 C49 C48 121.5(3) . . ?
C49 C50 H50 118.9 . . ?
C51 C50 C49 122.2(3) . . ?
C51 C50 H50 118.9 . . ?
O8 C51 C50 123.7(3) . . ?
O8 C51 C52 114.0(3) . . ?
C50 C51 C52 122.3(3) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C54 C53 C39 118.5(3) . . ?
C58 C53 C39 123.6(3) . . ?
C58 C53 C54 117.8(3) . . ?
C53 C54 H54 119.6 . . ?
C55 C54 C53 120.9(3) . . ?
C55 C54 H54 119.6 . . ?
C54 C55 H55 119.8 . . ?
C56 C55 C54 120.3(3) . . ?
C56 C55 H55 119.8 . . ?
C55 C56 H56 120.2 . . ?
C55 C56 C57 119.5(3) . . ?
C57 C56 H56 120.2 . . ?
C56 C57 H57 119.9 . . ?
C58 C57 C56 120.1(3) . . ?
C58 C57 H57 119.9 . . ?
C53 C58 H58 119.3 . . ?
C57 C58 C53 121.3(3) . . ?
C57 C58 H58 119.3 . . ?
C60 C59 C40 118.2(3) . . ?
C64 C59 C40 123.5(3) . . ?
C64 C59 C60 118.3(3) . . ?
C59 C60 H60 119.1 . . ?
C61 C60 C59 121.8(3) . . ?
C61 C60 H60 119.1 . . ?
C60 C61 H61 120.2 . . ?
C60 C61 C62 119.7(3) . . ?
C62 C61 H61 120.2 . . ?
C61 C62 H62 120.3 . . ?
C61 C62 C63 119.4(3) . . ?
C63 C62 H62 120.3 . . ?
C62 C63 H63 119.5 . . ?
C62 C63 C64 121.0(3) . . ?
C64 C63 H63 119.5 . . ?
C59 C64 C63 119.8(3) . . ?
C59 C64 H64 120.1 . . ?
C63 C64 H64 120.1 . . ?
C66 C65 C41 121.1(3) . . ?
C70 C65 C41 121.0(3) . . ?
C70 C65 C66 117.7(3) . . ?
C65 C66 H66 119.3 . . ?
C67 C66 C65 121.4(3) . . ?
C67 C66 H66 119.3 . . ?
C66 C67 H67 120.0 . . ?
C66 C67 C68 120.1(3) . . ?
C68 C67 H67 120.0 . . ?
C67 C68 H68 120.6 . . ?
C69 C68 C67 118.8(3) . . ?
C69 C68 H68 120.6 . . ?
C68 C69 H69 119.4 . . ?
C68 C69 C70 121.2(3) . . ?
C70 C69 H69 119.4 . . ?
C65 C70 H70 119.7 . . ?
C69 C70 C65 120.7(3) . . ?
C69 C70 H70 119.7 . . ?
C72 C71 C42 120.3(3) . . ?
C72 C71 C76 117.7(3) . . ?
C76 C71 C42 121.7(3) . . ?
C71 C72 H72 119.7 . . ?
C73 C72 C71 120.7(3) . . ?
C73 C72 H72 119.7 . . ?
C72 C73 H73 119.8 . . ?
C74 C73 C72 120.4(3) . . ?
C74 C73 H73 119.8 . . ?
C73 C74 H74 120.1 . . ?
C75 C74 C73 119.7(3) . . ?
C75 C74 H74 120.1 . . ?
C74 C75 H75 119.9 . . ?
C74 C75 C76 120.1(3) . . ?
C76 C75 H75 119.9 . . ?
C71 C76 H76 119.3 . . ?
C75 C76 C71 121.4(3) . . ?
C75 C76 H76 119.3 . . ?
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
Cl2 C77 1.784(5) . ?
C77 D77 1.0000 . ?
C77 D77A 1.0000 . ?
C77 Cl1A 1.722(7) . ?
C77 Cl3A 1.789(6) . ?
C77 Cl1B 1.876(12) . ?
C77 Cl3B 1.595(16) . ?
Cl5 C78 1.757(4) . ?
C78 D78 1.0000 . ?
C78 D78A 1.0000 . ?
C78 Cl4A 1.709(6) . ?
C78 Cl5A 1.792(5) . ?
C78 Cl4B 1.961(17) . ?
C78 Cl5B 1.599(11) . ?
Si1 O1 1.845(2) . ?
Si1 O2 1.839(2) . ?
Si1 O3 1.836(2) . ?
Si1 O4 1.820(2) . ?
Si1 C1 1.936(3) . ?
Si1 C4 1.926(3) . ?
O1 C5 1.282(4) . ?
O2 C7 1.293(4) . ?
O3 C10 1.277(4) . ?
O4 C12 1.277(4) . ?
C1 C2 1.348(4) . ?
C1 C15 1.478(4) . ?
C2 C3 1.506(4) . ?
C2 C21 1.489(4) . ?
C3 C4 1.356(4) . ?
C3 C27 1.487(4) . ?
C4 C33 1.485(4) . ?
C5 C6 1.384(5) . ?
C5 C8 1.498(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.383(4) . ?
C7 C9 1.501(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.386(5) . ?
C10 C13 1.502(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.393(5) . ?
C12 C14 1.496(5) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.392(4) . ?
C15 C20 1.412(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.397(5) . ?
C17 H17 0.9500 . ?
C17 C18 1.391(5) . ?
C18 H18 0.9500 . ?
C18 C19 1.381(5) . ?
C19 H19 0.9500 . ?
C19 C20 1.393(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.403(4) . ?
C21 C26 1.385(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.397(5) . ?
C23 H23 0.9500 . ?
C23 C24 1.375(6) . ?
C24 H24 0.9500 . ?
C24 C25 1.392(6) . ?
C25 H25 0.9500 . ?
C25 C26 1.399(5) . ?
C26 H26 0.9500 . ?
C27 C28 1.405(4) . ?
C27 C32 1.402(4) . ?
C28 H28 0.9500 . ?
C28 C29 1.381(5) . ?
C29 H29 0.9500 . ?
C29 C30 1.389(5) . ?
C30 H30 0.9500 . ?
C30 C31 1.402(5) . ?
C31 H31 0.9500 . ?
C31 C32 1.381(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.394(5) . ?
C33 C38 1.402(4) . ?
C34 H34 0.9500 . ?
C34 C35 1.396(5) . ?
C35 H35 0.9500 . ?
C35 C36 1.382(5) . ?
C36 H36 0.9500 . ?
C36 C37 1.385(6) . ?
C37 H37 0.9500 . ?
C37 C38 1.392(5) . ?
C38 H38 0.9500 . ?
Si2 O5 1.846(2) . ?
Si2 O6 1.840(2) . ?
Si2 O7 1.836(2) . ?
Si2 O8 1.824(2) . ?
Si2 C39 1.935(3) . ?
Si2 C42 1.924(3) . ?
O5 C43 1.286(4) . ?
O6 C45 1.284(4) . ?
O7 C49 1.285(4) . ?
O8 C51 1.290(4) . ?
C39 C40 1.353(4) . ?
C39 C53 1.483(4) . ?
C40 C41 1.502(4) . ?
C40 C59 1.493(4) . ?
C41 C42 1.350(4) . ?
C41 C65 1.493(4) . ?
C42 C71 1.479(4) . ?
C43 C44 1.394(5) . ?
C43 C46 1.484(4) . ?
C44 H44 0.9500 . ?
C44 C45 1.392(4) . ?
C45 C47 1.487(5) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C48 C49 1.496(4) . ?
C49 C50 1.390(5) . ?
C50 H50 0.9500 . ?
C50 C51 1.379(5) . ?
C51 C52 1.492(4) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 C54 1.406(4) . ?
C53 C58 1.395(4) . ?
C54 H54 0.9500 . ?
C54 C55 1.389(5) . ?
C55 H55 0.9500 . ?
C55 C56 1.386(5) . ?
C56 H56 0.9500 . ?
C56 C57 1.391(5) . ?
C57 H57 0.9500 . ?
C57 C58 1.387(5) . ?
C58 H58 0.9500 . ?
C59 C60 1.400(4) . ?
C59 C64 1.392(4) . ?
C60 H60 0.9500 . ?
C60 C61 1.380(5) . ?
C61 H61 0.9500 . ?
C61 C62 1.385(5) . ?
C62 H62 0.9500 . ?
C62 C63 1.388(5) . ?
C63 H63 0.9500 . ?
C63 C64 1.396(5) . ?
C64 H64 0.9500 . ?
C65 C66 1.402(4) . ?
C65 C70 1.398(4) . ?
C66 H66 0.9500 . ?
C66 C67 1.388(5) . ?
C67 H67 0.9500 . ?
C67 C68 1.397(5) . ?
C68 H68 0.9500 . ?
C68 C69 1.383(5) . ?
C69 H69 0.9500 . ?
C69 C70 1.390(5) . ?
C70 H70 0.9500 . ?
C71 C72 1.397(5) . ?
C71 C76 1.398(4) . ?
C72 H72 0.9500 . ?
C72 C73 1.397(5) . ?
C73 H73 0.9500 . ?
C73 C74 1.384(6) . ?
C74 H74 0.9500 . ?
C74 C75 1.377(6) . ?
C75 H75 0.9500 . ?
C75 C76 1.390(5) . ?
C76 H76 0.9500 . ?
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 O1 C5 C6 -14.4(4) . . . . ?
Si1 O1 C5 C8 166.7(2) . . . . ?
Si1 O2 C7 C6 13.6(4) . . . . ?
Si1 O2 C7 C9 -167.9(2) . . . . ?
Si1 O3 C10 C11 5.5(5) . . . . ?
Si1 O3 C10 C13 -173.9(2) . . . . ?
Si1 O4 C12 C11 -4.6(5) . . . . ?
Si1 O4 C12 C14 175.3(3) . . . . ?
Si1 C1 C2 C3 -7.7(3) . . . . ?
Si1 C1 C2 C21 169.3(2) . . . . ?
Si1 C1 C15 C16 59.3(4) . . . . ?
Si1 C1 C15 C20 -119.5(3) . . . . ?
Si1 C4 C33 C34 -111.8(3) . . . . ?
Si1 C4 C33 C38 66.5(4) . . . . ?
O1 Si1 O2 C7 -24.8(2) . . . . ?
O1 Si1 O3 C10 175.8(3) . . . . ?
O1 C5 C6 C7 -6.7(5) . . . . ?
O2 Si1 O1 C5 25.3(3) . . . . ?
O2 Si1 O3 C10 -92.8(3) . . . . ?
O2 Si1 O4 C12 91.7(3) . . . . ?
O3 Si1 O1 C5 109.9(3) . . . . ?
O3 Si1 O2 C7 -108.3(2) . . . . ?
O3 Si1 O4 C12 7.2(3) . . . . ?
O3 C10 C11 C12 0.1(5) . . . . ?
O4 Si1 O2 C7 159.6(2) . . . . ?
O4 Si1 O3 C10 -7.7(3) . . . . ?
C1 Si1 O1 C5 -68.9(3) . . . . ?
C1 Si1 O2 C7 68.0(2) . . . . ?
C1 Si1 O4 C12 -174.3(3) . . . . ?
C1 C2 C3 C4 4.8(4) . . . . ?
C1 C2 C3 C27 -169.5(3) . . . . ?
C1 C2 C21 C22 58.3(4) . . . . ?
C1 C2 C21 C26 -118.6(3) . . . . ?
C1 C15 C16 C17 -179.4(3) . . . . ?
C1 C15 C20 C19 179.2(3) . . . . ?
C2 C1 C15 C16 -124.9(3) . . . . ?
C2 C1 C15 C20 56.2(4) . . . . ?
C2 C3 C4 Si1 0.8(3) . . . . ?
C2 C3 C4 C33 -172.4(3) . . . . ?
C2 C3 C27 C28 44.8(4) . . . . ?
C2 C3 C27 C32 -139.8(3) . . . . ?
C2 C21 C22 C23 -176.1(3) . . . . ?
C2 C21 C26 C25 176.3(3) . . . . ?
C3 C2 C21 C22 -124.9(3) . . . . ?
C3 C2 C21 C26 58.2(4) . . . . ?
C3 C4 C33 C34 60.5(4) . . . . ?
C3 C4 C33 C38 -121.2(3) . . . . ?
C3 C27 C28 C29 171.3(3) . . . . ?
C3 C27 C32 C31 -172.2(3) . . . . ?
C4 Si1 O1 C5 -156.1(3) . . . . ?
C4 Si1 O3 C10 86.2(3) . . . . ?
C4 Si1 O4 C12 -86.9(3) . . . . ?
C4 C3 C27 C28 -128.9(3) . . . . ?
C4 C3 C27 C32 46.4(4) . . . . ?
C4 C33 C34 C35 178.9(3) . . . . ?
C4 C33 C38 C37 179.8(3) . . . . ?
C5 C6 C7 O2 7.1(5) . . . . ?
C5 C6 C7 C9 -171.3(3) . . . . ?
C8 C5 C6 C7 172.1(3) . . . . ?
C10 C11 C12 O4 -0.5(5) . . . . ?
C10 C11 C12 C14 179.6(3) . . . . ?
C13 C10 C11 C12 179.4(3) . . . . ?
C15 C1 C2 C3 176.0(3) . . . . ?
C15 C1 C2 C21 -7.1(5) . . . . ?
C15 C16 C17 C18 0.2(5) . . . . ?
C16 C15 C20 C19 0.3(5) . . . . ?
C16 C17 C18 C19 0.2(5) . . . . ?
C17 C18 C19 C20 -0.4(5) . . . . ?
C18 C19 C20 C15 0.1(5) . . . . ?
C20 C15 C16 C17 -0.5(5) . . . . ?
C21 C2 C3 C4 -172.3(3) . . . . ?
C21 C2 C3 C27 13.5(4) . . . . ?
C21 C22 C23 C24 -0.4(5) . . . . ?
C22 C21 C26 C25 -0.7(5) . . . . ?
C22 C23 C24 C25 -0.2(5) . . . . ?
C23 C24 C25 C26 0.4(6) . . . . ?
C24 C25 C26 C21 0.1(5) . . . . ?
C26 C21 C22 C23 0.9(5) . . . . ?
C27 C3 C4 Si1 174.9(2) . . . . ?
C27 C3 C4 C33 1.7(5) . . . . ?
C27 C28 C29 C30 1.6(5) . . . . ?
C28 C27 C32 C31 3.3(5) . . . . ?
C28 C29 C30 C31 2.1(5) . . . . ?
C29 C30 C31 C32 -3.0(5) . . . . ?
C30 C31 C32 C27 0.3(5) . . . . ?
C32 C27 C28 C29 -4.3(4) . . . . ?
C33 C34 C35 C36 0.8(5) . . . . ?
C34 C33 C38 C37 -1.8(5) . . . . ?
C34 C35 C36 C37 -1.0(6) . . . . ?
C35 C36 C37 C38 -0.3(5) . . . . ?
C36 C37 C38 C33 1.7(5) . . . . ?
C38 C33 C34 C35 0.6(5) . . . . ?
Si2 O5 C43 C44 17.1(4) . . . . ?
Si2 O5 C43 C46 -164.4(2) . . . . ?
Si2 O6 C45 C44 -16.1(4) . . . . ?
Si2 O6 C45 C47 165.6(2) . . . . ?
Si2 O7 C49 C48 176.4(2) . . . . ?
Si2 O7 C49 C50 -2.8(5) . . . . ?
Si2 O8 C51 C50 1.0(5) . . . . ?
Si2 O8 C51 C52 -178.8(2) . . . . ?
Si2 C39 C40 C41 9.6(3) . . . . ?
Si2 C39 C40 C59 -166.5(2) . . . . ?
Si2 C39 C53 C54 -59.5(4) . . . . ?
Si2 C39 C53 C58 120.0(3) . . . . ?
Si2 C42 C71 C72 97.4(3) . . . . ?
Si2 C42 C71 C76 -77.4(4) . . . . ?
O5 Si2 O6 C45 27.3(3) . . . . ?
O5 Si2 O7 C49 177.7(3) . . . . ?
O5 C43 C44 C45 4.7(5) . . . . ?
O6 Si2 O5 C43 -27.8(3) . . . . ?
O6 Si2 O7 C49 86.5(3) . . . . ?
O6 Si2 O8 C51 -85.1(3) . . . . ?
O7 Si2 O5 C43 -112.7(3) . . . . ?
O7 Si2 O6 C45 110.7(2) . . . . ?
O7 Si2 O8 C51 -0.3(3) . . . . ?
O7 C49 C50 C51 3.2(5) . . . . ?
O8 Si2 O6 C45 -157.2(3) . . . . ?
O8 Si2 O7 C49 1.2(3) . . . . ?
C39 Si2 O5 C43 66.3(3) . . . . ?
C39 Si2 O6 C45 -65.3(3) . . . . ?
C39 Si2 O8 C51 -179.1(3) . . . . ?
C39 C40 C41 C42 -6.9(4) . . . . ?
C39 C40 C41 C65 167.4(3) . . . . ?
C39 C40 C59 C60 116.3(3) . . . . ?
C39 C40 C59 C64 -60.9(4) . . . . ?
C39 C53 C54 C55 -179.5(3) . . . . ?
C39 C53 C58 C57 179.6(3) . . . . ?
C40 C39 C53 C54 125.0(3) . . . . ?
C40 C39 C53 C58 -55.5(4) . . . . ?
C40 C41 C42 Si2 0.3(3) . . . . ?
C40 C41 C42 C71 170.7(3) . . . . ?
C40 C41 C65 C66 -43.5(4) . . . . ?
C40 C41 C65 C70 140.7(3) . . . . ?
C40 C59 C60 C61 -175.8(3) . . . . ?
C40 C59 C64 C63 176.5(3) . . . . ?
C41 C40 C59 C60 -59.7(4) . . . . ?
C41 C40 C59 C64 123.1(3) . . . . ?
C41 C42 C71 C72 -71.9(4) . . . . ?
C41 C42 C71 C76 113.4(4) . . . . ?
C41 C65 C66 C67 -171.8(3) . . . . ?
C41 C65 C70 C69 172.0(3) . . . . ?
C42 Si2 O5 C43 153.9(3) . . . . ?
C42 Si2 O7 C49 -92.2(3) . . . . ?
C42 Si2 O8 C51 93.3(3) . . . . ?
C42 C41 C65 C66 130.3(3) . . . . ?
C42 C41 C65 C70 -45.5(4) . . . . ?
C42 C71 C72 C73 -176.4(3) . . . . ?
C42 C71 C76 C75 177.5(3) . . . . ?
C43 C44 C45 O6 -5.2(5) . . . . ?
C43 C44 C45 C47 173.0(3) . . . . ?
C46 C43 C44 C45 -173.7(3) . . . . ?
C48 C49 C50 C51 -175.9(3) . . . . ?
C49 C50 C51 O8 -2.3(5) . . . . ?
C49 C50 C51 C52 177.5(3) . . . . ?
C53 C39 C40 C41 -174.2(3) . . . . ?
C53 C39 C40 C59 9.6(5) . . . . ?
C53 C54 C55 C56 -0.5(5) . . . . ?
C54 C53 C58 C57 -0.9(5) . . . . ?
C54 C55 C56 C57 -0.1(5) . . . . ?
C55 C56 C57 C58 0.1(5) . . . . ?
C56 C57 C58 C53 0.4(5) . . . . ?
C58 C53 C54 C55 1.0(5) . . . . ?
C59 C40 C41 C42 169.4(3) . . . . ?
C59 C40 C41 C65 -16.3(4) . . . . ?
C59 C60 C61 C62 -1.3(5) . . . . ?
C60 C59 C64 C63 -0.7(5) . . . . ?
C60 C61 C62 C63 0.3(5) . . . . ?
C61 C62 C63 C64 0.4(5) . . . . ?
C62 C63 C64 C59 -0.2(5) . . . . ?
C64 C59 C60 C61 1.5(5) . . . . ?
C65 C41 C42 Si2 -173.8(2) . . . . ?
C65 C41 C42 C71 -3.5(5) . . . . ?
C65 C66 C67 C68 -1.5(5) . . . . ?
C66 C65 C70 C69 -4.0(5) . . . . ?
C66 C67 C68 C69 -1.5(5) . . . . ?
C67 C68 C69 C70 1.7(5) . . . . ?
C68 C69 C70 C65 1.1(5) . . . . ?
C70 C65 C66 C67 4.2(4) . . . . ?
C71 C72 C73 C74 -0.6(6) . . . . ?
C72 C71 C76 C75 2.6(5) . . . . ?
C72 C73 C74 C75 1.6(6) . . . . ?
C73 C74 C75 C76 -0.4(5) . . . . ?
C74 C75 C76 C71 -1.8(5) . . . . ?
C76 C71 C72 C73 -1.4(5) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.609(11)
2 0.391(11)
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
1.2191 8.6946 -0.5301 -0.1501 -0.0301 0.9882
5.2035 0.1652 7.8208 -0.9830 -0.1832 -0.0088
-4.0140 -6.3129 -4.3449 0.7010 0.1321 -0.7008
-3.4081 5.9782 -6.7835 0.7003 0.1290 0.7021
4.5979 4.4656 -10.7384 0.0651 -0.7983 0.5987
5.1397 -3.2407 -11.2245 0.0760 -0.9619 -0.2626
-2.3170 -7.8394 5.9404 -0.0305 0.3551 -0.9343
-4.3113 5.6455 9.1384 -0.0649 0.8316 0.5516
0.9980 8.7242 0.3298 -0.1732 0.0247 0.9846
-2.4693 4.9300 -10.0898 0.7849 -0.1013 0.6114
-2.7357 -6.5166 -6.9890 0.7085 -0.0940 -0.6994
-0.7350 -8.7758 0.5790 0.0960 -0.0146 -0.9953
2.3117 -5.3792 9.7128 -0.7450 0.0959 -0.6601
3.4184 2.8155 10.5964 -0.9570 0.1256 0.2616
-0.2311 8.8129 -0.4634 0.0011 0.1107 0.9939
-4.5318 5.8850 7.9943 0.0194 0.8106 0.5853
-5.7180 -1.9353 11.0445 0.0244 0.9466 -0.3216
-0.0745 -8.8033 1.0422 0.0002 -0.0591 -0.9983
5.6833 -2.7067 -10.5036 -0.0243 -0.9785 -0.2047
4.6480 5.2028 -9.3492 -0.0198 -0.7399 0.6724
