#------------------------------------------------------------------------------
#$Date: 2024-07-05 17:05:04 +0200 (Fri 05 de Jul de 2024) $
#$Revision: 292913 $
#$URL: svn://www.crystallography.net/cod/cif/1/57/13/1571349.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_1571349
loop_
_publ_author_name
'Tricoire, Maxime'
'Hsueh, Fang-Che'
'Keener, Megan'
'Rajeshkumar, Thayalan'
'Scopelliti, Rosario'
'Zivkovic, Ivica'
'Maron, Laurent'
'Mazzanti, Marinella'
_publ_section_title
;
 Siloxide tripodal ligands as a scaffold for stabilizing lanthanides in
 the +4 oxidation state.
;
_journal_issue                   18
_journal_name_full               'Chemical science'
_journal_page_first              6874
_journal_page_last               6883
_journal_paper_doi               10.1039/d4sc00051j
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety
'C66 H84 Ce O10 Si4, 0.5(C20 H40 K O5), 0.5(C24 H48 K0.949 O6), 2.7[C4H8O]'
_chemical_formula_sum            'C88 H128 Ce K O15.5 Si4'
_chemical_formula_weight         1725.48
_space_group_crystal_system      hexagonal
_space_group_IT_number           182
_space_group_name_Hall           'P 6c 2c'
_space_group_name_H-M_alt        'P 63 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-24
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.17 svn.r577a77a9 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-09-22 deposited with the CCDC.	2024-03-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            4
_cell_length_a                   14.87393(16)
_cell_length_b                   14.87393(16)
_cell_length_c                   55.4259(7)
_cell_measurement_reflns_used    35991
_cell_measurement_temperature    200.00(11)
_cell_measurement_theta_max      72.3610
_cell_measurement_theta_min      3.1220
_cell_volume                     10619.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.80a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.80a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.80a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -68.00 -15.00   1.00    1.50    --  -43.01 113.00  27.00   53
  2  ω    -90.00  32.00   1.00    1.50    --  -43.01  17.00 -77.00  122
  3  ω    117.00 162.00   1.00    6.00    --  103.49  17.00 -77.00   45
  4  ω     62.00  87.00   1.00    6.00    --  103.49 -17.00 113.00   25
  5  ω    132.00 158.00   1.00    6.00    --  103.49 110.00  90.00   26
  6  ω     77.00 139.00   1.00    6.00    --  103.49 157.00 159.00   62
  7  ω    139.00 165.00   1.00    6.00    --  103.49 113.00  27.00   26
  8  ω     97.00 174.00   1.00    6.00    --  103.49 128.00 -21.00   77
  9  ω     69.00  94.00   1.00    6.00    --  103.49-113.00 -64.00   25
 10  ω    109.00 134.00   1.00    6.00    --  103.49 138.00 -46.00   25
 11  ω     71.00  97.00   1.00    6.00    --  103.49  17.00 -77.00   26
 12  ω    -42.00 -15.00   1.00    1.50    --  -43.01 -57.00   0.00   27
 13  ω    -44.00 -19.00   1.00    1.50    --  -43.01 -57.00 -60.00   25
 14  ω    -51.00 -26.00   1.00    1.50    --  -43.01 -57.00 -30.00   25
 15  ω     20.00  53.00   1.00    1.50    --   43.01  37.00   0.00   33
 16  ω     10.00  37.00   1.00    1.50    --   43.01  79.00  64.13   27
 17  ω     73.00  98.00   1.00    6.00    --  103.49  70.00  36.09   25
 18  ω     73.00  99.00   1.00    6.00    --  103.49  67.00  26.14   26
 19  ω     74.00 100.00   1.00    6.00    --  103.49  61.00  30.00   26
 20  ω     75.00 102.00   1.00    6.00    --  103.49  61.00  60.00   27
 21  ω     78.00 173.00   1.00    6.00    --  103.49  59.00  39.75   95
 22  ω     74.00 100.00   1.00    6.00    --  103.49  61.00   0.00   26
 23  ω     76.00 102.00   1.00    6.00    --  103.49  57.00  11.27   26
 24  ω     78.00 105.00   1.00    6.00    --  103.49  45.00   0.00   27
 25  ω     76.00 116.00   1.00    6.00    --  103.49  56.00  30.03   40
 26  ω     74.00 100.00   1.00    6.00    --  103.49  64.00  50.68   26
 27  ω     75.00 100.00   1.00    6.00    --  103.49  60.00 -10.06   25
 28  ω     77.00 121.00   1.00    6.00    --  103.49  60.00  12.54   44
 29  ω     80.00 107.00   1.00    6.00    --  103.49  47.00  10.13   27
 30  ω     73.00 100.00   1.00    6.00    --  103.49  69.00   5.70   27
 31  ω     77.00 159.00   1.00    6.00    --  103.49  61.00 -30.00   82
 32  ω     74.00  99.00   1.00    6.00    --  103.49  67.00  43.52   25
 33  ω     71.00 104.00   1.00    6.00    --  103.49-110.00  -4.00   33
;
_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      -0.0257956000
_diffrn_orient_matrix_UB_12      -0.1115223000
_diffrn_orient_matrix_UB_13      0.0060002000
_diffrn_orient_matrix_UB_21      0.1167132000
_diffrn_orient_matrix_UB_22      0.0372398000
_diffrn_orient_matrix_UB_23      0.0021059000
_diffrn_orient_matrix_UB_31      -0.0032308000
_diffrn_orient_matrix_UB_32      0.0217965000
_diffrn_orient_matrix_UB_33      0.0270734000
_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  0.0379
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       68
_diffrn_reflns_limit_l_min       -62
_diffrn_reflns_number            86994
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.678
_diffrn_reflns_theta_min         3.189
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.508
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.218
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.80a (Rigaku Oxford Diffraction, 2023)
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 pale colourless'
_exptl_crystal_density_diffrn    1.079
_exptl_crystal_description       prism
_exptl_crystal_F_000             3652
_exptl_crystal_size_max          0.411
_exptl_crystal_size_mid          0.277
_exptl_crystal_size_min          0.229
_refine_diff_density_max         0.909
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.071(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         7038
_refine_ls_number_restraints     551
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0581
_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)+(0.0731P)²+17.4658P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1554
_refine_ls_wR_factor_ref         0.1561
_reflns_Friedel_coverage         0.669
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                6906
_reflns_number_total             7038
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4sc00051j2.cif
_cod_data_source_block           ah543
_cod_depositor_comments
'Adding full bibliography for 1571342--1571354.cif.'
_cod_original_cell_volume        10619.3(3)
_cod_original_formula_sum        'C88 H128 Ce K O15.50 Si4'
_cod_database_code               1571349
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C88 H128 O15.5 Si4 K1 Ce1'
_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.
;
_shelx_estimated_absorpt_t_max   0.425
_shelx_estimated_absorpt_t_min   0.259
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.929(10)
 0.071(10)
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
 O6-C33 = O6-C30
 1.44 with sigma of 0.02
 C32-C31
 1.54 with sigma of 0.02
 C33-C32 = C31-C30
 1.53 with sigma of 0.02
 C26-C27 = C28-C29
 1.53 with sigma of 0.02
 O5-C26 = O5-C29
 1.44 with sigma of 0.02
 C27-C28
 1.54 with sigma of 0.02
 O6-C32 = O6-C31 = C33-C31 = C32-C30
 2.38 with sigma of 0.04
 O5-C27 = O5-C28 = C26-C28 = C27-C29
 2.38 with sigma of 0.04
 C15-C9 \\sim C12-C9 \\sim C11-C9 \\sim C14-C9 \\sim C10-C9 \\sim C13-C9
 with sigma of 0.02
 C14-C15 \\sim C15-C13
 with sigma of 0.02
 C10-C11 \\sim C11-C12
 with sigma of 0.02
 C32-C30 \\sim C33-C31
 with sigma of 0.04
 O6-C32 \\sim O6-C31
 with sigma of 0.04
 O6-C33 \\sim O6-C30
 with sigma of 0.02
 C33-C32 \\sim C32-C31 \\sim C31-C30
 with sigma of 0.02
 C26-C27 \\sim C27-C28 \\sim C28-C29
 with sigma of 0.02
 O5-C26 \\sim O5-C29
 with sigma of 0.02
 O5-C27 \\sim O5-C28
 with sigma of 0.04
 C27-C29 \\sim C26-C28
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O6 \\sim C30 \\sim C31 \\sim C32 \\sim C33: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O5 \\sim C26 \\sim C27 \\sim C28 \\sim C29: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 O6, C30, C31, C32, C33
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, C26, C27, C28, C29
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=1-FVAR(1)
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(1)
 Fixed Sof: O5(0.5) O6(0.333333) C26(0.5) H26A(0.5) H26B(0.5) C27(0.5)
 H27A(0.5) H27B(0.5) C28(0.5) H28A(0.5) H28B(0.5) C29(0.5) H29A(0.5) H29B(0.5)
 C30(0.333333) H30A(0.333333) H30B(0.333333) C31(0.333333) H31A(0.333333)
 H31B(0.333333) C32(0.333333) H32A(0.333333) H32B(0.333333) C33(0.333333)
 H33A(0.333333) H33B(0.333333)
7.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,
 H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B),
 C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C5(H5), C6(H6), C7(H7), C21(H21), C22(H22), C23(H23),
 C24(H24), C25(H25)
7.c Fitted pentagon refined as free rotating group:
 O7(C34,C35,C36,C37)
7.d Fitted hexagon refined as free rotating group:
 C20(C21,C22,C23,C24,C25)
7.e Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,
 H18B,H18C), C19(H19A,H19B,H19C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 410 electrons were 
found in a volume of 1878Å³ in 2 voids per unit cell. 
This is consistent with the presence of 
2.7[C4H8O] per Asymmetric Unit 
which account for 432 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_date_sample_data_collection 2023-01-25
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.464
_oxdiff_exptl_absorpt_empirical_full_min 0.767
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-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
Ce1 Ce 0.333333 0.666667 0.61533(2) 0.03908(17) Uani 1 3 d S T P . .
Si1 Si 0.18541(16) 0.79816(17) 0.59647(3) 0.0472(4) Uani 1 1 d . . . . .
Si2 Si 0.333333 0.666667 0.68391(5) 0.0614(7) Uani 1 3 d S T P . .
O1 O 0.2453(5) 0.7505(5) 0.60990(7) 0.0548(10) Uani 1 1 d . . . . .
O2 O 0.0734(4) 0.7148(4) 0.58491(9) 0.0596(11) Uani 1 1 d . . . . .
O3 O 0.1635(4) 0.8745(4) 0.61406(8) 0.0575(11) Uani 1 1 d . . . . .
O4 O 0.333333 0.666667 0.65530(14) 0.070(2) Uani 1 3 d S T P . .
C1 C 0.4235(5) 0.7635(5) 0.55624(11) 0.0398(12) Uani 1 1 d . . . . .
H1 H 0.484632 0.829796 0.556654 0.048 Uiso 1 1 calc R U . . .
C2 C 0.3249(6) 0.7561(5) 0.55593(11) 0.0413(12) Uani 1 1 d . . . . .
C3 C 0.3215(5) 0.8553(5) 0.55419(11) 0.0433(11) Uani 1 1 d . . . . .
C4 C 0.3781(6) 0.9234(5) 0.53561(13) 0.0536(15) Uani 1 1 d . . . . .
H4 H 0.416686 0.905754 0.524898 0.064 Uiso 1 1 calc R U . . .
C5 C 0.3792(7) 1.0160(6) 0.53246(15) 0.070(2) Uani 1 1 d . . . . .
H5 H 0.419535 1.062311 0.519944 0.083 Uiso 1 1 calc R U . . .
C6 C 0.3218(9) 1.0406(7) 0.54748(15) 0.077(2) Uani 1 1 d . . . . .
H6 H 0.320562 1.103250 0.545220 0.093 Uiso 1 1 calc R U . . .
C7 C 0.2658(7) 0.9738(6) 0.56595(14) 0.065(2) Uani 1 1 d . . . . .
H7 H 0.227849 0.992792 0.576527 0.078 Uiso 1 1 calc R U . . .
C8 C 0.2627(5) 0.8802(5) 0.56971(12) 0.0474(12) Uani 1 1 d . . . . .
C9 C -0.0170(6) 0.6304(7) 0.59564(16) 0.0733(18) Uani 1 1 d D U . . .
C10 C -0.1094(11) 0.6309(15) 0.5841(3) 0.087(4) Uani 0.599(10) 1 d D U P A 1
H10A H -0.103865 0.698714 0.586657 0.131 Uiso 0.599(10) 1 calc R U P A 1
H10B H -0.173690 0.576618 0.591448 0.131 Uiso 0.599(10) 1 calc R U P A 1
H10C H -0.110232 0.617775 0.566755 0.131 Uiso 0.599(10) 1 calc R U P A 1
C11 C -0.0256(12) 0.6430(14) 0.6229(3) 0.095(4) Uani 0.599(10) 1 d D U P A 1
H11A H 0.021648 0.626146 0.631527 0.143 Uiso 0.599(10) 1 calc R U P A 1
H11B H -0.097086 0.595924 0.628201 0.143 Uiso 0.599(10) 1 calc R U P A 1
H11C H -0.007021 0.714784 0.626460 0.143 Uiso 0.599(10) 1 calc R U P A 1
C12 C -0.0129(15) 0.5329(11) 0.5918(4) 0.095(4) Uani 0.599(10) 1 d D U P A 1
H12A H -0.019303 0.516592 0.574495 0.143 Uiso 0.599(10) 1 calc R U P A 1
H12B H -0.070064 0.475561 0.600512 0.143 Uiso 0.599(10) 1 calc R U P A 1
H12C H 0.053445 0.542659 0.597737 0.143 Uiso 0.599(10) 1 calc R U P A 1
C13 C -0.0721(17) 0.566(2) 0.5733(4) 0.094(5) Uani 0.401(10) 1 d D U P A 2
H13A H -0.102772 0.600085 0.564107 0.141 Uiso 0.401(10) 1 calc R U P A 2
H13B H -0.126849 0.496580 0.578245 0.141 Uiso 0.401(10) 1 calc R U P A 2
H13C H -0.021733 0.559141 0.563090 0.141 Uiso 0.401(10) 1 calc R U P A 2
C14 C -0.0846(16) 0.6737(18) 0.6035(5) 0.080(4) Uani 0.401(10) 1 d D U P A 2
H14A H -0.065652 0.701129 0.619974 0.120 Uiso 0.401(10) 1 calc R U P A 2
H14B H -0.157562 0.618567 0.603214 0.120 Uiso 0.401(10) 1 calc R U P A 2
H14C H -0.074670 0.729668 0.592577 0.120 Uiso 0.401(10) 1 calc R U P A 2
C15 C 0.0122(18) 0.5760(18) 0.6145(4) 0.092(5) Uani 0.401(10) 1 d D U P A 2
H15A H 0.054765 0.550185 0.607092 0.138 Uiso 0.401(10) 1 calc R U P A 2
H15B H -0.050910 0.517613 0.621267 0.138 Uiso 0.401(10) 1 calc R U P A 2
H15C H 0.051771 0.624993 0.627436 0.138 Uiso 0.401(10) 1 calc R U P A 2
C16 C 0.2121(7) 0.9292(7) 0.63532(15) 0.0676(16) Uani 1 1 d . . . . .
C17 C 0.3272(8) 0.9966(8) 0.63128(17) 0.083(2) Uani 1 1 d . . . . .
H17A H 0.358589 0.952706 0.629484 0.124 Uiso 1 1 calc R U . . .
H17B H 0.358395 1.043053 0.645123 0.124 Uiso 1 1 calc R U . . .
H17C H 0.339377 1.037966 0.616615 0.124 Uiso 1 1 calc R U . . .
C18 C 0.1929(8) 0.8547(8) 0.65593(15) 0.084(2) Uani 1 1 d . . . . .
H18A H 0.118736 0.803413 0.656818 0.127 Uiso 1 1 calc R U . . .
H18B H 0.215299 0.893397 0.671129 0.127 Uiso 1 1 calc R U . . .
H18C H 0.232414 0.819031 0.653167 0.127 Uiso 1 1 calc R U . . .
C19 C 0.1618(9) 0.9959(8) 0.64043(19) 0.095(3) Uani 1 1 d . . . . .
H19A H 0.160220 1.030667 0.625556 0.142 Uiso 1 1 calc R U . . .
H19B H 0.202363 1.048059 0.652699 0.142 Uiso 1 1 calc R U . . .
H19C H 0.090792 0.951390 0.646299 0.142 Uiso 1 1 calc R U . . .
C20 C 0.3734(5) 0.7990(4) 0.69615(11) 0.0682(18) Uani 1 1 d G . . . .
C21 C 0.4402(5) 0.8850(5) 0.68242(11) 0.101(3) Uani 1 1 d G . . . .
H21 H 0.465283 0.875918 0.667391 0.121 Uiso 1 1 calc R U . . .
C22 C 0.4702(6) 0.9844(4) 0.69068(16) 0.126(4) Uani 1 1 d G . . . .
H22 H 0.515898 1.043151 0.681299 0.152 Uiso 1 1 calc R U . . .
C23 C 0.4335(7) 0.9977(5) 0.71268(18) 0.144(4) Uani 1 1 d G . . . .
H23 H 0.454060 1.065586 0.718324 0.173 Uiso 1 1 calc R U . . .
C24 C 0.3667(8) 0.9117(7) 0.72641(14) 0.165(7) Uani 1 1 d G . . . .
H24 H 0.341608 0.920788 0.741442 0.198 Uiso 1 1 calc R U . . .
C25 C 0.3366(6) 0.8123(6) 0.71815(11) 0.119(4) Uani 1 1 d G . . . .
H25 H 0.290992 0.753554 0.727534 0.142 Uiso 1 1 calc R U . . .
K1 K 0.000000 1.000000 0.500000 0.328(11) Uani 1 6 d S T P . .
O5 O -0.0211(19) 0.8019(18) 0.5035(8) 0.168(10) Uani 0.5 1 d D U P B -1
O6 O -0.0545(16) 0.960(2) 0.5425(5) 0.130(7) Uani 0.3333 1 d D U P B -1
C26 C -0.079(2) 0.693(3) 0.4979(9) 0.181(12) Uani 0.5 1 d D U P B -1
H26A H -0.124398 0.681672 0.483680 0.218 Uiso 0.5 1 calc R U P B -1
H26B H -0.123747 0.653892 0.511694 0.218 Uiso 0.5 1 calc R U P B -1
C27 C -0.002(3) 0.660(2) 0.4925(6) 0.161(10) Uani 0.5 1 d D U P B -1
H27A H -0.030986 0.584585 0.495768 0.193 Uiso 0.5 1 calc R U P B -1
H27B H 0.022315 0.674500 0.475588 0.193 Uiso 0.5 1 calc R U P B -1
C28 C 0.083(2) 0.725(2) 0.5097(7) 0.155(10) Uani 0.5 1 d D U P B -1
H28A H 0.076122 0.685943 0.524832 0.186 Uiso 0.5 1 calc R U P B -1
H28B H 0.151911 0.746051 0.502511 0.186 Uiso 0.5 1 calc R U P B -1
C29 C 0.071(2) 0.816(2) 0.5146(7) 0.160(9) Uani 0.5 1 d D U P B -1
H29A H 0.068353 0.825154 0.532178 0.192 Uiso 0.5 1 calc R U P B -1
H29B H 0.132009 0.879339 0.508040 0.192 Uiso 0.5 1 calc R U P B -1
C30 C 0.016(4) 0.936(4) 0.5547(6) 0.149(10) Uani 0.3333 1 d D U P B -1
H30A H 0.088537 0.984703 0.549848 0.178 Uiso 0.3333 1 calc R U P B -1
H30B H -0.000490 0.864242 0.551148 0.178 Uiso 0.3333 1 calc R U P B -1
C31 C -0.001(4) 0.949(5) 0.5813(5) 0.136(10) Uani 0.3333 1 d D U P B -1
H31A H 0.062204 0.966357 0.590934 0.163 Uiso 0.3333 1 calc R U P B -1
H31B H -0.060499 0.885298 0.587945 0.163 Uiso 0.3333 1 calc R U P B -1
C32 C -0.022(4) 1.039(4) 0.5802(6) 0.140(9) Uani 0.3333 1 d D U P B -1
H32A H -0.058819 1.041636 0.594804 0.168 Uiso 0.3333 1 calc R U P B -1
H32B H 0.043559 1.106477 0.578431 0.168 Uiso 0.3333 1 calc R U P B -1
C33 C -0.089(3) 1.014(3) 0.5579(7) 0.122(7) Uani 0.3333 1 d D U P B -1
H33A H -0.163714 0.969550 0.561963 0.146 Uiso 0.3333 1 calc R U P B -1
H33B H -0.079388 1.078215 0.550005 0.146 Uiso 0.3333 1 calc R U P B -1
K2 K 0.000000 1.000000 0.750000 0.0886(12) Uani 1 6 d S T P . .
O7 O -0.0151(11) 0.8458(7) 0.72274(17) 0.166(4) Uani 1 1 d G . . . .
C34 C -0.0999(11) 0.7887(13) 0.7068(3) 0.227(8) Uani 1 1 d G U . . .
H34A H -0.093513 0.831214 0.692501 0.272 Uiso 1 1 calc R U . . .
H34B H -0.166109 0.769911 0.715087 0.272 Uiso 1 1 calc R U . . .
C35 C -0.0986(13) 0.6977(11) 0.6998(3) 0.257(13) Uani 1 1 d G . . . .
H35A H -0.164127 0.635192 0.704611 0.309 Uiso 1 1 calc R U . . .
H35B H -0.091529 0.696496 0.682025 0.309 Uiso 1 1 calc R U . . .
C36 C -0.0129(16) 0.6984(11) 0.7113(4) 0.267(14) Uani 1 1 d G . . . .
H36A H 0.035163 0.697563 0.699055 0.320 Uiso 1 1 calc R U . . .
H36B H -0.037435 0.636261 0.721641 0.320 Uiso 1 1 calc R U . . .
C37 C 0.0386(11) 0.7899(12) 0.7255(3) 0.259(14) Uani 1 1 d G . . . .
H37A H 0.111481 0.832942 0.720055 0.311 Uiso 1 1 calc R U . . .
H37B H 0.038884 0.771640 0.742641 0.311 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'
Ce Ce -1.8482 9.6596 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.3868 1.0657 '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 -1 -2 0.1811
1 1 2 0.2158
1 1 -1 0.2198
2 2 -1 0.2214
-2 -2 1 0.1886
0 1 0 0.2105
0 1 1 0.2025
0 2 -1 0.2122
0 1 2 0.1924
0 -1 -1 0.2025
0 -2 1 0.2057
0 0 1 0.1149
-1 2 2 0.1761
-1 2 0 0.1705
-1 2 -1 0.1747
1 -1 -1 0.1275
1 -1 0 0.1296
1 -1 1 0.1328
1 -1 2 0.1308
-1 1 1 0.1459
-1 1 0 0.1463
-2 2 -1 0.1450
-1 1 -1 0.1459
-1 1 -2 0.1456
2 -1 -2 0.1601
1 0 2 0.1854
-2 0 1 0.1738
2 0 -1 0.1954
7 -2 -22 0.1636
-5 -1 -27 0.1497
2 2 34 0.1322
-2 2 35 0.1198
-5 2 30 0.1276
5 2 -24 0.1810
-1 -4 -30 0.1422
-3 0 33 0.1275
-2 1 35 0.1151
0 3 33 0.1338
-1 -3 33 0.1251
1 -5 -29 0.1343
0 6 -24 0.1934
-1 4 32 0.1336
1 -2 -35 0.1083
-5 8 -20 0.1592
4 -6 29 0.1138
6 -9 3 0.1488
3 -5 -30 0.1214
-4 7 26 0.1389
-6 5 -27 0.1318
-4 5 30 0.1214
4 -3 33 0.1182
6 -6 -26 0.1178
-5 0 -30 0.1311
-10 3 0 0.1646
-5 3 30 0.1202
-8 9 1 0.1403
-6 7 -22 0.1408
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 Ce1 O1 118.22(5) 3_565 2_665 ?
O1 Ce1 O1 118.22(5) . 2_665 ?
O1 Ce1 O1 118.22(5) . 3_565 ?
O4 Ce1 O1 97.73(10) . 2_665 ?
O4 Ce1 O1 97.73(10) . 3_565 ?
O4 Ce1 O1 97.73(10) . . ?
O1 Si1 O2 115.9(3) . . ?
O1 Si1 O3 112.4(2) . . ?
O1 Si1 C8 111.2(3) . . ?
O2 Si1 O3 106.1(3) . . ?
O2 Si1 C8 104.0(3) . . ?
O3 Si1 C8 106.5(3) . . ?
O4 Si2 C20 111.2(2) . . ?
O4 Si2 C20 111.2(2) . 3_565 ?
O4 Si2 C20 111.2(2) . 2_665 ?
C20 Si2 C20 107.7(2) . 3_565 ?
C20 Si2 C20 107.7(2) 2_665 3_565 ?
C20 Si2 C20 107.7(2) . 2_665 ?
Si1 O1 Ce1 159.3(3) . . ?
C9 O2 Si1 131.2(5) . . ?
C16 O3 Si1 132.3(5) . . ?
Si2 O4 Ce1 180.0 . . ?
C2 C1 H1 119.9 . . ?
C2 C1 H1 119.9 3_565 . ?
C2 C1 C2 120.2(7) 3_565 . ?
C1 C2 C1 119.7(7) 2_665 . ?
C1 C2 C3 117.8(7) . . ?
C1 C2 C3 122.4(7) 2_665 . ?
C4 C3 C2 117.2(6) . . ?
C4 C3 C8 119.3(6) . . ?
C8 C3 C2 123.5(6) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 C3 121.4(7) . . ?
C5 C4 H4 119.3 . . ?
C4 C5 H5 120.3 . . ?
C6 C5 C4 119.5(7) . . ?
C6 C5 H5 120.3 . . ?
C5 C6 H6 120.2 . . ?
C5 C6 C7 119.5(7) . . ?
C7 C6 H6 120.2 . . ?
C6 C7 H7 118.6 . . ?
C6 C7 C8 122.7(7) . . ?
C8 C7 H7 118.6 . . ?
C3 C8 Si1 124.4(5) . . ?
C7 C8 Si1 118.0(5) . . ?
C7 C8 C3 117.5(7) . . ?
O2 C9 C10 106.0(9) . . ?
O2 C9 C11 113.7(9) . . ?
O2 C9 C12 108.3(8) . . ?
O2 C9 C13 100.8(11) . . ?
O2 C9 C14 106.4(11) . . ?
O2 C9 C15 111.2(11) . . ?
C10 C9 C11 106.4(10) . . ?
C12 C9 C10 114.8(13) . . ?
C12 C9 C11 107.8(11) . . ?
C14 C9 C13 104.1(16) . . ?
C14 C9 C15 117.4(13) . . ?
C15 C9 C13 115.5(14) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C13 H13A 109.5 . . ?
C9 C13 H13B 109.5 . . ?
C9 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C9 C14 H14A 109.5 . . ?
C9 C14 H14B 109.5 . . ?
C9 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C9 C15 H15A 109.5 . . ?
C9 C15 H15B 109.5 . . ?
C9 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O3 C16 C17 110.1(7) . . ?
O3 C16 C18 110.7(7) . . ?
O3 C16 C19 104.6(7) . . ?
C17 C16 C18 109.5(8) . . ?
C17 C16 C19 110.8(8) . . ?
C18 C16 C19 111.0(8) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 Si2 118.3(4) . . ?
C21 C20 C25 120.0 . . ?
C25 C20 Si2 121.7(4) . . ?
C20 C21 H21 120.0 . . ?
C20 C21 C22 120.0 . . ?
C22 C21 H21 120.0 . . ?
C21 C22 H22 120.0 . . ?
C23 C22 C21 120.0 . . ?
C23 C22 H22 120.0 . . ?
C22 C23 H23 120.0 . . ?
C22 C23 C24 120.0 . . ?
C24 C23 H23 120.0 . . ?
C23 C24 H24 120.0 . . ?
C25 C24 C23 120.0 . . ?
C25 C24 H24 120.0 . . ?
C20 C25 H25 120.0 . . ?
C24 C25 C20 120.0 . . ?
C24 C25 H25 120.0 . . ?
O5 K1 C29 23.0(5) . . ?
O5 K1 C30 67.1(12) . . ?
O5 K1 C33 98.7(11) . . ?
O6 K1 O5 80.2(12) . . ?
O6 K1 C29 77.4(10) . . ?
O6 K1 C30 24.9(6) . . ?
O6 K1 C33 19.1(8) . . ?
C29 K1 C33 96.2(9) . . ?
C30 K1 C29 57.0(9) . . ?
C30 K1 C33 41.0(8) . . ?
C26 O5 K1 148(2) . . ?
C29 O5 K1 106.4(16) . . ?
C29 O5 C26 105(2) . . ?
C30 O6 K1 109(2) . . ?
C30 O6 C33 112(2) . . ?
C33 O6 K1 127(2) . . ?
O5 C26 H26A 110.4 . . ?
O5 C26 H26B 110.4 . . ?
O5 C26 C27 107(2) . . ?
H26A C26 H26B 108.6 . . ?
C27 C26 H26A 110.4 . . ?
C27 C26 H26B 110.4 . . ?
C26 C27 H27A 111.5 . . ?
C26 C27 H27B 111.5 . . ?
H27A C27 H27B 109.3 . . ?
C28 C27 C26 101.6(15) . . ?
C28 C27 H27A 111.5 . . ?
C28 C27 H27B 111.5 . . ?
C27 C28 H28A 110.7 . . ?
C27 C28 H28B 110.7 . . ?
H28A C28 H28B 108.8 . . ?
C29 C28 C27 105.0(14) . . ?
C29 C28 H28A 110.7 . . ?
C29 C28 H28B 110.7 . . ?
K1 C29 H29A 93.9 . . ?
K1 C29 H29B 70.1 . . ?
O5 C29 K1 50.6(13) . . ?
O5 C29 C28 109.7(17) . . ?
O5 C29 H29A 109.7 . . ?
O5 C29 H29B 109.7 . . ?
C28 C29 K1 154(2) . . ?
C28 C29 H29A 109.7 . . ?
C28 C29 H29B 109.7 . . ?
H29A C29 H29B 108.2 . . ?
K1 C30 H30A 75.1 . . ?
K1 C30 H30B 96.7 . . ?
O6 C30 K1 46.5(15) . . ?
O6 C30 H30A 110.9 . . ?
O6 C30 H30B 110.9 . . ?
O6 C30 C31 104(2) . . ?
H30A C30 H30B 108.9 . . ?
C31 C30 K1 147(2) . . ?
C31 C30 H30A 110.9 . . ?
C31 C30 H30B 110.9 . . ?
C30 C31 H31A 111.6 . . ?
C30 C31 H31B 111.6 . . ?
C30 C31 C32 101(2) . . ?
H31A C31 H31B 109.4 . . ?
C32 C31 H31A 111.6 . . ?
C32 C31 H31B 111.6 . . ?
C31 C32 H32A 111.3 . . ?
C31 C32 H32B 111.3 . . ?
H32A C32 H32B 109.2 . . ?
C33 C32 C31 103(2) . . ?
C33 C32 H32A 111.3 . . ?
C33 C32 H32B 111.3 . . ?
K1 C33 H33A 119.9 . . ?
K1 C33 H33B 77.2 . . ?
O6 C33 K1 34.2(17) . . ?
O6 C33 C32 104(2) . . ?
O6 C33 H33A 111.0 . . ?
O6 C33 H33B 111.0 . . ?
C32 C33 K1 122(2) . . ?
C32 C33 H33A 111.0 . . ?
C32 C33 H33B 111.0 . . ?
H33A C33 H33B 109.0 . . ?
O7 K2 O7 90.9(3) . 2_675 ?
O7 K2 O7 83.4(5) 2_675 10_666 ?
O7 K2 O7 95.3(6) 3_465 11_456 ?
O7 K2 O7 83.4(5) 12_576 3_465 ?
O7 K2 O7 90.9(3) 11_456 10_666 ?
O7 K2 O7 90.9(3) 12_576 11_456 ?
O7 K2 O7 83.4(5) . 11_456 ?
O7 K2 O7 95.3(6) . 10_666 ?
O7 K2 O7 90.9(3) 12_576 10_666 ?
O7 K2 O7 95.3(6) 12_576 2_675 ?
O7 K2 O7 171.6(6) 2_675 11_456 ?
O7 K2 O7 90.9(3) 3_465 2_675 ?
O7 K2 O7 171.6(6) . 12_576 ?
O7 K2 O7 90.9(3) . 3_465 ?
O7 K2 O7 171.6(6) 3_465 10_666 ?
C34 O7 K2 122.3(8) . . ?
C34 O7 C37 108.0 . . ?
C37 O7 K2 127.9(8) . . ?
O7 C34 H34A 110.1 . . ?
O7 C34 H34B 110.1 . . ?
O7 C34 C35 108.0 . . ?
H34A C34 H34B 108.4 . . ?
C35 C34 H34A 110.1 . . ?
C35 C34 H34B 110.1 . . ?
C34 C35 H35A 110.1 . . ?
C34 C35 H35B 110.1 . . ?
H35A C35 H35B 108.4 . . ?
C36 C35 C34 108.0 . . ?
C36 C35 H35A 110.1 . . ?
C36 C35 H35B 110.1 . . ?
C35 C36 H36A 110.1 . . ?
C35 C36 H36B 110.1 . . ?
C35 C36 C37 108.0 . . ?
H36A C36 H36B 108.4 . . ?
C37 C36 H36A 110.1 . . ?
C37 C36 H36B 110.1 . . ?
O7 C37 H37A 110.1 . . ?
O7 C37 H37B 110.1 . . ?
C36 C37 O7 108.0 . . ?
C36 C37 H37A 110.1 . . ?
C36 C37 H37B 110.1 . . ?
H37A C37 H37B 108.4 . . ?
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
Ce1 O1 2.235(4) . ?
Ce1 O1 2.235(4) 2_665 ?
Ce1 O1 2.235(4) 3_565 ?
Ce1 O4 2.216(8) . ?
Si1 O1 1.575(4) . ?
Si1 O2 1.630(6) . ?
Si1 O3 1.647(5) . ?
Si1 C8 1.899(7) . ?
Si2 O4 1.586(8) . ?
Si2 C20 1.876(5) . ?
Si2 C20 1.876(5) 2_665 ?
Si2 C20 1.875(5) 3_565 ?
O2 C9 1.432(10) . ?
O3 C16 1.409(10) . ?
C1 H1 0.9500 . ?
C1 C2 1.415(8) . ?
C1 C2 1.376(8) 3_565 ?
C2 C3 1.504(8) . ?
C3 C4 1.394(9) . ?
C3 C8 1.403(9) . ?
C4 H4 0.9500 . ?
C4 C5 1.380(10) . ?
C5 H5 0.9500 . ?
C5 C6 1.366(11) . ?
C6 H6 0.9500 . ?
C6 C7 1.378(11) . ?
C7 H7 0.9500 . ?
C7 C8 1.385(9) . ?
C9 C10 1.519(14) . ?
C9 C11 1.537(14) . ?
C9 C12 1.498(14) . ?
C9 C13 1.532(17) . ?
C9 C14 1.505(16) . ?
C9 C15 1.514(16) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
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 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.506(13) . ?
C16 C18 1.517(12) . ?
C16 C19 1.538(12) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.3900 . ?
C20 C25 1.3900 . ?
C21 H21 0.9500 . ?
C21 C22 1.3900 . ?
C22 H22 0.9500 . ?
C22 C23 1.3900 . ?
C23 H23 0.9500 . ?
C23 C24 1.3900 . ?
C24 H24 0.9500 . ?
C24 C25 1.3900 . ?
C25 H25 0.9500 . ?
K1 O5 2.81(2) . ?
K1 O6 2.46(3) . ?
K1 C29 3.49(3) . ?
K1 C30 3.22(4) . ?
K1 C33 3.52(4) . ?
O5 C26 1.432(19) . ?
O5 C29 1.421(18) . ?
O6 C30 1.43(2) . ?
O6 C33 1.44(2) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.501(18) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.492(17) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.481(17) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.521(18) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.532(18) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.520(18) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
K2 O7 2.661(8) . ?
K2 O7 2.661(8) 10_666 ?
K2 O7 2.661(8) 12_576 ?
K2 O7 2.661(8) 2_675 ?
K2 O7 2.661(8) 3_465 ?
K2 O7 2.661(8) 11_456 ?
O7 C34 1.4200 . ?
O7 C37 1.4200 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.4200 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.4200 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C37 1.4200 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
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 O2 C9 C10 141.1(9) . . . . ?
Si1 O2 C9 C11 24.5(12) . . . . ?
Si1 O2 C9 C12 -95.2(11) . . . . ?
Si1 O2 C9 C13 -160.0(12) . . . . ?
Si1 O2 C9 C14 91.8(13) . . . . ?
Si1 O2 C9 C15 -37.1(13) . . . . ?
Si1 O3 C16 C17 53.8(10) . . . . ?
Si1 O3 C16 C18 -67.4(9) . . . . ?
Si1 O3 C16 C19 172.9(6) . . . . ?
Si2 C20 C21 C22 178.9(5) . . . . ?
Si2 C20 C25 C24 -178.9(5) . . . . ?
O1 Si1 O2 C9 55.5(7) . . . . ?
O1 Si1 O3 C16 22.3(8) . . . . ?
O1 Si1 C8 C3 38.5(7) . . . . ?
O1 Si1 C8 C7 -137.9(6) . . . . ?
O2 Si1 O1 Ce1 68.1(12) . . . . ?
O2 Si1 O3 C16 149.9(7) . . . . ?
O2 Si1 C8 C3 -86.9(6) . . . . ?
O2 Si1 C8 C7 96.7(7) . . . . ?
O3 Si1 O1 Ce1 -169.6(10) . . . . ?
O3 Si1 O2 C9 -70.0(6) . . . . ?
O3 Si1 C8 C3 161.3(6) . . . . ?
O3 Si1 C8 C7 -15.2(7) . . . . ?
O4 Si2 C20 C21 -28.9(4) . . . . ?
O4 Si2 C20 C25 150.0(4) . . . . ?
C1 C2 C3 C4 -125.5(8) 2_665 . . . ?
C1 C2 C3 C4 51.9(9) . . . . ?
C1 C2 C3 C8 -130.0(7) . . . . ?
C1 C2 C3 C8 52.7(10) 2_665 . . . ?
C2 C1 C2 C1 2.4(14) 3_565 . . 2_665 ?
C2 C1 C2 C3 -175.0(4) 3_565 . . . ?
C2 C3 C4 C5 179.6(7) . . . . ?
C2 C3 C8 Si1 4.1(10) . . . . ?
C2 C3 C8 C7 -179.4(7) . . . . ?
C3 C4 C5 C6 -1.5(14) . . . . ?
C4 C3 C8 Si1 -177.7(5) . . . . ?
C4 C3 C8 C7 -1.3(10) . . . . ?
C4 C5 C6 C7 1.7(15) . . . . ?
C5 C6 C7 C8 -1.7(16) . . . . ?
C6 C7 C8 Si1 178.2(8) . . . . ?
C6 C7 C8 C3 1.5(13) . . . . ?
C8 Si1 O1 Ce1 -50.3(12) . . . . ?
C8 Si1 O2 C9 177.9(6) . . . . ?
C8 Si1 O3 C16 -99.8(7) . . . . ?
C8 C3 C4 C5 1.3(11) . . . . ?
C20 Si2 C20 C21 93.2(5) 3_565 . . . ?
C20 Si2 C20 C21 -151.0(4) 2_665 . . . ?
C20 Si2 C20 C25 -87.9(4) 3_565 . . . ?
C20 Si2 C20 C25 27.9(5) 2_665 . . . ?
C20 C21 C22 C23 0.0 . . . . ?
C21 C20 C25 C24 0.0 . . . . ?
C21 C22 C23 C24 0.0 . . . . ?
C22 C23 C24 C25 0.0 . . . . ?
C23 C24 C25 C20 0.0 . . . . ?
C25 C20 C21 C22 0.0 . . . . ?
K1 O5 C26 C27 142(5) . . . . ?
K1 O5 C29 C28 -161(3) . . . . ?
K1 O6 C30 C31 162(3) . . . . ?
K1 O6 C33 C32 -128(3) . . . . ?
K1 C30 C31 C32 -10(9) . . . . ?
O5 C26 C27 C28 35(5) . . . . ?
O6 C30 C31 C32 -35(5) . . . . ?
C26 O5 C29 K1 176(4) . . . . ?
C26 O5 C29 C28 15(5) . . . . ?
C26 C27 C28 C29 -25(5) . . . . ?
C27 C28 C29 K1 -29(8) . . . . ?
C27 C28 C29 O5 7(5) . . . . ?
C29 O5 C26 C27 -32(5) . . . . ?
C30 O6 C33 K1 137(4) . . . . ?
C30 O6 C33 C32 9(5) . . . . ?
C30 C31 C32 C33 40(5) . . . . ?
C31 C32 C33 K1 -62(5) . . . . ?
C31 C32 C33 O6 -31(5) . . . . ?
C33 O6 C30 K1 -145(3) . . . . ?
C33 O6 C30 C31 17(5) . . . . ?
K2 O7 C34 C35 -165.6(9) . . . . ?
K2 O7 C37 C36 164.6(10) . . . . ?
O7 C34 C35 C36 0.0 . . . . ?
C34 O7 C37 C36 0.0 . . . . ?
C34 C35 C36 C37 0.0 . . . . ?
C35 C36 C37 O7 0.0 . . . . ?
C37 O7 C34 C35 0.0 . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.929(10)
2 0.071(10)
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
-1.0028 -0.9972 -2.0303 0.1249 -0.1585 -0.0735
1.0028 0.9972 2.0303 -0.1249 0.1585 0.0735
1.0016 1.0018 -0.9694 -0.1434 0.1522 -0.0076
2.0037 2.0020 -0.9389 -0.2806 0.3064 0.0117
-2.0037 -2.0020 0.9389 0.2806 -0.3064 -0.0117
-0.0007 1.0006 0.0151 -0.1115 0.0372 0.0222
-0.0003 0.9991 1.0150 -0.1053 0.0393 0.0493
-0.0018 2.0028 -0.9696 -0.2291 0.0723 0.0174
0.0000 0.9976 2.0149 -0.0992 0.0414 0.0763
0.0003 -0.9991 -1.0150 0.1053 -0.0393 -0.0493
0.0018 -2.0028 0.9696 0.2291 -0.0723 -0.0174
0.0004 -0.0015 0.9999 0.0062 0.0021 0.0270
-1.0034 1.9986 2.0146 -0.1849 -0.0384 0.1013
-1.0042 2.0016 0.0149 -0.1972 -0.0426 0.0473
-1.0046 2.0031 -0.9850 -0.2034 -0.0447 0.0202
1.0031 -0.9995 -0.9996 0.0796 0.0778 -0.0521
1.0035 -1.0010 0.0003 0.0857 0.0798 -0.0251
1.0039 -1.0025 1.0001 0.0919 0.0819 0.0020
1.0043 -1.0040 2.0000 0.0981 0.0840 0.0290
-1.0031 0.9995 0.9996 -0.0796 -0.0778 0.0521
-1.0035 1.0010 -0.0003 -0.0857 -0.0798 0.0251
-2.0074 2.0035 -1.0004 -0.1777 -0.1618 0.0231
-1.0039 1.0025 -1.0001 -0.0919 -0.0819 -0.0020
-1.0043 1.0040 -2.0000 -0.0981 -0.0840 -0.0290
2.0055 -0.9983 -1.9841 0.0477 0.1927 -0.0820
1.0035 -0.0034 2.0151 -0.0134 0.1212 0.0512
-2.0051 -0.0008 0.9691 0.0576 -0.2320 0.0327
2.0051 0.0008 -0.9691 -0.0576 0.2320 -0.0327
7.2232 -1.6439 -22.3526 -0.1371 0.7348 -0.6643
-4.6108 -1.4683 -27.0887 0.1201 -0.6499 -0.7505
1.5117 1.9803 33.5037 -0.0588 0.3207 0.9453
-1.8668 2.1960 34.8704 0.0125 -0.0627 0.9980
-5.1647 2.0485 30.3234 0.0867 -0.4626 0.8823
4.8836 2.2238 -23.6802 -0.5161 0.6029 -0.6084
-1.0102 -3.8969 -30.3389 0.2786 -0.3269 -0.9031
-3.4743 -0.0370 32.6874 0.2899 -0.3380 0.8954
-2.2983 1.2737 34.9327 0.1268 -0.1472 0.9809
0.1948 3.3715 32.7124 -0.1847 0.2172 0.9585
-0.8103 -2.6614 33.3183 0.5176 -0.1235 0.8466
1.4497 -5.3555 -29.4635 0.3831 -0.0923 -0.9191
0.1696 6.1899 -23.7581 -0.8372 0.2003 -0.5088
-1.4269 4.1317 32.3947 -0.2296 0.0555 0.9717
1.2916 -1.7205 -35.3416 -0.0535 0.0123 -0.9985
-5.2686 7.9481 -19.6271 -0.8682 -0.3603 -0.3411
3.7262 -5.5495 29.1228 0.6975 0.2896 0.6555
6.2137 -9.4679 3.1359 0.9144 0.3792 -0.1415
3.4061 -5.3382 -29.8186 0.3285 0.1360 -0.9347
-4.1907 6.5187 26.2535 -0.4614 -0.1911 0.8664
-5.9393 4.7752 -27.2428 -0.5428 -0.5727 -0.6143
-4.2884 4.8087 30.1385 -0.2448 -0.2580 0.9346
3.7163 -2.5511 33.0369 0.3869 0.4083 0.8268
5.5945 -5.9123 -26.1053 0.3584 0.3778 -0.8537
-4.6722 0.1718 -30.0406 -0.0789 -0.6022 -0.7945
-9.5200 3.3523 -0.1866 -0.1294 -0.9867 0.0988
-5.4812 3.3870 29.5043 -0.0593 -0.4515 0.8903
-7.5915 8.9658 0.6193 -0.8003 -0.5508 0.2367
-6.2009 6.9270 -22.0908 -0.7451 -0.5123 -0.4271
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.175 8.2 0.0 ?
2 0.000 0.000 0.325 8.2 0.0 ?
3 0.000 0.000 0.675 8.2 0.0 ?
4 0.000 0.000 0.825 8.2 0.0 ?
5 0.333 0.667 0.250 922.8 204.6 '5.4 thf'
6 0.667 0.333 0.750 922.8 208.5 '5.4 thf'
