#------------------------------------------------------------------------------
#$Date: 2023-07-05 12:40:56 +0300 (Wed, 05 Jul 2023) $
#$Revision: 284891 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/90/1569057.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_1569057
loop_
_publ_author_name
'Hsueh, Fang-Che'
'Rajeshkumar, Thayalan'
'Maron, Laurent'
'Scopelliti, Rosario'
'Sienkiewicz, Andrzej'
'Mazzanti, Marinella'
_publ_section_title
;
 Isolation and redox reactivity of cerium complexes in four redox states.
;
_journal_issue                   22
_journal_name_full               'Chemical science'
_journal_page_first              6011
_journal_page_last               6021
_journal_paper_doi               10.1039/d3sc01478a
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C60 H99 Ce K2 O12 Si3'
_chemical_formula_sum            'C60 H99 Ce K2 O12 Si3'
_chemical_formula_weight         1314.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-11-19
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-01 deposited with the CCDC.	2023-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.250(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.2554(11)
_cell_length_b                   11.0935(6)
_cell_length_c                   25.7721(14)
_cell_measurement_reflns_used    3760
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.1220
_cell_measurement_theta_min      3.5930
_cell_volume                     6966.3(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_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)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -9.00  29.00   1.00   10.00    --  -40.91  82.00  34.00   38
  2  ω     96.00 127.00   1.00   40.00    --  105.15 -82.00 -87.00   31
  3  ω     49.00  76.00   1.00   40.00    --  105.15 -82.00 -87.00   27
  4  ω    116.00 141.00   1.00   40.00    --  105.15  82.00  34.00   25
  5  ω     46.00  73.00   1.00   10.00    --   40.91 -77.00  30.00   27
  6  ω     36.00 112.00   1.00   10.00    --   40.91  38.00 120.00   76
  7  ω      7.00  58.00   1.00   10.00    --   40.91 -99.00-180.00   51
  8  ω    -21.00  33.00   1.00   10.00    --   40.91 -77.00  30.00   54
  9  ω    -17.00  73.00   1.00   10.00    --   40.91 -82.00 -87.00   90
 10  ω    104.00 177.00   1.00   40.00    --  105.15 111.00   0.00   73
 11  ω     35.00 122.00   1.00   40.00    --  105.15 -45.00 -30.00   87
 12  ω     54.00  96.00   1.00   40.00    --  105.15-111.00-150.00   42
 13  ω    111.00 177.00   1.00   40.00    --  105.15 111.00 -90.00   66
 14  ω     70.00 112.00   1.00   40.00    --  105.15 -30.00 -60.00   42
 15  ω    129.00 177.00   1.00   40.00    --  105.15 111.00  90.00   48
 16  ω     29.00  57.00   1.00   40.00    --  105.15 -30.00 -60.00   28
 17  ω    119.00 176.00   1.00   40.00    --  105.15 111.00  30.00   57
 18  ω    104.00 178.00   1.00   40.00    --  105.15 111.00-120.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0400461000
_diffrn_orient_matrix_UB_12      0.1073929000
_diffrn_orient_matrix_UB_13      -0.0101258000
_diffrn_orient_matrix_UB_21      -0.0303053000
_diffrn_orient_matrix_UB_22      -0.0540449000
_diffrn_orient_matrix_UB_23      -0.0548332000
_diffrn_orient_matrix_UB_31      -0.0385008000
_diffrn_orient_matrix_UB_32      -0.0694327000
_diffrn_orient_matrix_UB_33      0.0269229000
_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  0.1266
_diffrn_reflns_av_unetI/netI     0.1546
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            35961
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.786
_diffrn_reflns_theta_min         3.555
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.035
_exptl_absorpt_correction_T_max  0.790
_exptl_absorpt_correction_T_min  0.285
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent dark purple'
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_description       plate
_exptl_crystal_F_000             2772
_exptl_crystal_size_max          0.287
_exptl_crystal_size_mid          0.052
_exptl_crystal_size_min          0.046
_refine_diff_density_max         1.351
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     809
_refine_ls_number_reflns         13487
_refine_ls_number_restraints     240
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1349
_refine_ls_R_factor_gt           0.0762
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0719P)²+4.0848P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1703
_refine_ls_wR_factor_ref         0.2000
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8102
_reflns_number_total             13487
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3sc01478a2.cif
_cod_data_source_block           ah499-4
_cod_depositor_comments
'Adding full bibliography for 1569056--1569065.cif.'
_cod_database_code               1569057
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C63.5 H103 O12 Si3 K2 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   0.738
_shelx_estimated_absorpt_t_min   0.237
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C36-C34 \\sim C40-C34 \\sim C37-C34 \\sim C38-C34 \\sim C35-C34 \\sim C39-C34
 with sigma of 0.02
 C36-C37 \\sim C37-C35 \\sim C35-C36
 with sigma of 0.02
 C39-C40 \\sim C40-C38 \\sim C38-C39
 with sigma of 0.02
 C63-C64 \\sim C67-C68 \\sim C66-C65
 with sigma of 0.02
 O12-C67 \\sim O12-C65 \\sim O12-C63
 with sigma of 0.02
 C21-C22 \\sim C22-C23 \\sim C21-C23
 with sigma of 0.02
 C20-C19 \\sim C19-C18 \\sim C18-C20
 with sigma of 0.02
 C20-C17 \\sim C21-C17 \\sim C18-C17 \\sim C22-C17 \\sim C19-C17 \\sim C23-C17
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O12 \\sim C65 \\sim C66 \\sim C67 \\sim C68: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Others
 Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=
 Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=1-FVAR(1)
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=FVAR(1)
 Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=1-FVAR(2)
 Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(H66C)=FVAR(2)
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=1-FVAR(3)
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(3)
5.a Ternary CH refined with riding coordinates:
 C2(H2), C4(H4), C6(H6)
5.b Secondary CH2 refined with riding coordinates:
 C55(H55A,H55B), C57(H57A,H57B), C59(H59A,H59B), C61(H61A,H61B), C63(H63A,
 H63B), C65(H65A,H65B), C67(H67A,H67B)
5.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C25(H25), C26(H26), C27(H27), C28(H28),
 C42(H42), C43(H43), C44(H44), C45(H45)
5.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,
 H22B,H22C), C23(H23A,H23B,H23C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C),
 C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,
 H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C48(H48A,
 H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C),
 C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C58(H58A,H58B,
 H58C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C), C64(H64A,H64B,H64C), C66(H66A,
 H66B,H66C), C68(H68A,H68B,H68C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 80 electrons were 
found in a volume of 410Å³ in 1 void per unit cell. 
This is consistent with the presence of 
0.4[C7H8] per Asymmetric Unit 
which account for 80 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_date_sample_data_collection 2022-11-16
_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 2.059
_oxdiff_exptl_absorpt_empirical_full_min 0.511
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, 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 0.54677(2) 0.70258(5) 0.33126(2) 0.02876(13) Uani 1 1 d . . . . .
K1 K 0.69956(7) 0.54061(19) 0.34743(8) 0.0398(4) Uani 1 1 d . . . . .
K2 K 0.43305(7) 0.6210(2) 0.20812(8) 0.0523(6) Uani 1 1 d . . . . .
Si1 Si 0.67238(8) 0.7473(2) 0.43609(9) 0.0303(5) Uani 1 1 d . . . . .
Si2 Si 0.56141(8) 0.5259(2) 0.21470(9) 0.0316(5) Uani 1 1 d . . . . .
Si3 Si 0.40922(8) 0.8322(2) 0.29297(9) 0.0331(5) Uani 1 1 d . . . . .
O1 O 0.6299(2) 0.6589(5) 0.3971(2) 0.0338(13) Uani 1 1 d . . . . .
O2 O 0.6855(2) 0.7091(6) 0.4996(2) 0.0393(14) Uani 1 1 d . . . . .
O3 O 0.7300(2) 0.7349(5) 0.4168(2) 0.0354(14) Uani 1 1 d . . . . .
O4 O 0.5369(2) 0.5528(5) 0.2647(2) 0.0307(12) Uani 1 1 d . . . . .
O5 O 0.5661(2) 0.3825(6) 0.2017(2) 0.0387(14) Uani 1 1 d . . . . .
O6 O 0.5138(2) 0.5739(6) 0.1614(2) 0.0363(14) Uani 1 1 d . . . . .
O7 O 0.4503(2) 0.7203(5) 0.3085(2) 0.0305(12) Uani 1 1 d . . . . .
O8 O 0.3442(2) 0.7905(6) 0.2743(2) 0.0442(15) Uani 1 1 d . . . . .
O9 O 0.4177(2) 0.9270(6) 0.3426(2) 0.0396(14) Uani 1 1 d . . . . .
O10 O 0.5111(2) 0.6142(6) 0.4129(2) 0.0380(14) Uani 1 1 d . . . . .
O11 O 0.7691(3) 0.3551(7) 0.3894(3) 0.0566(18) Uani 1 1 d . . . . .
O12 O 0.3546(3) 0.4668(7) 0.1529(4) 0.071(2) Uani 1 1 d D U . . .
C1 C 0.5963(3) 0.9245(8) 0.3379(3) 0.0311(18) Uani 1 1 d . . . . .
C2 C 0.6323(3) 0.8610(7) 0.3158(3) 0.0277(17) Uani 1 1 d . . . . .
H2 H 0.670511 0.847735 0.338583 0.033 Uiso 1 1 calc R U . . .
C3 C 0.6137(3) 0.7896(7) 0.2687(3) 0.0236(15) Uani 1 1 d . . . . .
C4 C 0.5585(3) 0.8154(7) 0.2364(3) 0.0281(17) Uani 1 1 d . . . . .
H4 H 0.544575 0.772656 0.201286 0.034 Uiso 1 1 calc R U . . .
C5 C 0.5227(3) 0.8897(8) 0.2546(3) 0.0333(19) Uani 1 1 d . . . . .
C6 C 0.5378(3) 0.9339(8) 0.3099(3) 0.0293(17) Uani 1 1 d . . . . .
H6 H 0.512522 0.986209 0.323977 0.035 Uiso 1 1 calc R U . . .
C7 C 0.6162(3) 0.9772(8) 0.3939(3) 0.0298(18) Uani 1 1 d . . . . .
C8 C 0.5974(3) 1.0901(8) 0.4026(4) 0.039(2) Uani 1 1 d . . . . .
H8 H 0.574000 1.132342 0.373315 0.047 Uiso 1 1 calc R U . . .
C9 C 0.6117(4) 1.1431(9) 0.4528(4) 0.045(2) Uani 1 1 d . . . . .
H9 H 0.598607 1.221500 0.457595 0.054 Uiso 1 1 calc R U . . .
C10 C 0.6447(4) 1.0833(10) 0.4958(4) 0.050(2) Uani 1 1 d . . . . .
H10 H 0.655513 1.119423 0.530422 0.060 Uiso 1 1 calc R U . . .
C11 C 0.6618(3) 0.9670(10) 0.4869(3) 0.042(2) Uani 1 1 d . . . . .
H11 H 0.683403 0.923805 0.516902 0.051 Uiso 1 1 calc R U . . .
C12 C 0.6493(3) 0.9109(8) 0.4371(3) 0.0300(18) Uani 1 1 d . . . . .
C13 C 0.6793(3) 0.5979(9) 0.5253(4) 0.037(2) Uani 1 1 d . . . . .
C14 C 0.6180(4) 0.5812(11) 0.5220(4) 0.060(3) Uani 1 1 d . . . . .
H14A H 0.604723 0.650783 0.538389 0.089 Uiso 1 1 calc R U . . .
H14B H 0.613016 0.507692 0.541341 0.089 Uiso 1 1 calc R U . . .
H14C H 0.597135 0.574341 0.484263 0.089 Uiso 1 1 calc R U . . .
C15 C 0.7101(4) 0.6129(11) 0.5839(4) 0.059(3) Uani 1 1 d . . . . .
H15A H 0.748860 0.629172 0.586713 0.088 Uiso 1 1 calc R U . . .
H15B H 0.706885 0.538803 0.603604 0.088 Uiso 1 1 calc R U . . .
H15C H 0.694370 0.680402 0.599419 0.088 Uiso 1 1 calc R U . . .
C16 C 0.6997(5) 0.4945(11) 0.5001(5) 0.063(3) Uani 1 1 d . . . . .
H16A H 0.678426 0.487396 0.462479 0.095 Uiso 1 1 calc R U . . .
H16B H 0.695861 0.420449 0.519449 0.095 Uiso 1 1 calc R U . . .
H16C H 0.738520 0.507173 0.501536 0.095 Uiso 1 1 calc R U . . .
C17 C 0.7861(3) 0.7762(8) 0.4392(3) 0.045(2) Uani 1 1 d D U . . .
C18 C 0.7883(5) 0.9013(11) 0.4609(5) 0.066(4) Uani 0.820(11) 1 d D U P A 1
H18A H 0.768834 0.904247 0.489102 0.099 Uiso 0.820(11) 1 calc R U P A 1
H18B H 0.770783 0.956725 0.431793 0.099 Uiso 0.820(11) 1 calc R U P A 1
H18C H 0.826628 0.925063 0.475893 0.099 Uiso 0.820(11) 1 calc R U P A 1
C19 C 0.8144(4) 0.6876(11) 0.4828(4) 0.051(3) Uani 0.820(11) 1 d D U P A 1
H19A H 0.853994 0.702680 0.492947 0.077 Uiso 0.820(11) 1 calc R U P A 1
H19B H 0.807257 0.605017 0.469237 0.077 Uiso 0.820(11) 1 calc R U P A 1
H19C H 0.800027 0.697959 0.514369 0.077 Uiso 0.820(11) 1 calc R U P A 1
C20 C 0.8142(4) 0.7690(12) 0.3938(5) 0.053(3) Uani 0.820(11) 1 d D U P A 1
H20A H 0.799273 0.831477 0.367074 0.079 Uiso 0.820(11) 1 calc R U P A 1
H20B H 0.807533 0.689441 0.376746 0.079 Uiso 0.820(11) 1 calc R U P A 1
H20C H 0.853720 0.781288 0.408297 0.079 Uiso 0.820(11) 1 calc R U P A 1
C21 C 0.782(2) 0.900(2) 0.4130(18) 0.054(7) Uani 0.180(11) 1 d D U P A 2
H21A H 0.770636 0.959756 0.436134 0.081 Uiso 0.180(11) 1 calc R U P A 2
H21B H 0.754760 0.898096 0.377949 0.081 Uiso 0.180(11) 1 calc R U P A 2
H21C H 0.817759 0.923380 0.407960 0.081 Uiso 0.180(11) 1 calc R U P A 2
C22 C 0.8010(19) 0.791(4) 0.4995(8) 0.056(7) Uani 0.180(11) 1 d D U P A 2
H22A H 0.825489 0.860786 0.509692 0.084 Uiso 0.180(11) 1 calc R U P A 2
H22B H 0.819710 0.718419 0.516606 0.084 Uiso 0.180(11) 1 calc R U P A 2
H22C H 0.767622 0.804273 0.511238 0.084 Uiso 0.180(11) 1 calc R U P A 2
C23 C 0.8261(16) 0.699(4) 0.4212(17) 0.048(6) Uani 0.180(11) 1 d D U P A 2
H23A H 0.817201 0.698355 0.381860 0.072 Uiso 0.180(11) 1 calc R U P A 2
H23B H 0.824050 0.616039 0.434207 0.072 Uiso 0.180(11) 1 calc R U P A 2
H23C H 0.863279 0.730047 0.435831 0.072 Uiso 0.180(11) 1 calc R U P A 2
C24 C 0.6487(3) 0.7058(8) 0.2518(3) 0.0338(18) Uani 1 1 d . . . . .
C25 C 0.7069(3) 0.7291(8) 0.2662(4) 0.039(2) Uani 1 1 d . . . . .
H25 H 0.720610 0.797522 0.287685 0.047 Uiso 1 1 calc R U . . .
C26 C 0.7435(3) 0.6552(9) 0.2497(4) 0.044(2) Uani 1 1 d . . . . .
H26 H 0.781419 0.674985 0.259386 0.053 Uiso 1 1 calc R U . . .
C27 C 0.7257(4) 0.5515(9) 0.2189(4) 0.046(2) Uani 1 1 d . . . . .
H27 H 0.750625 0.501589 0.206827 0.055 Uiso 1 1 calc R U . . .
C28 C 0.6700(3) 0.5251(9) 0.2067(4) 0.039(2) Uani 1 1 d . . . . .
H28 H 0.657499 0.455202 0.185718 0.047 Uiso 1 1 calc R U . . .
C29 C 0.6310(3) 0.5941(8) 0.2232(3) 0.0344(19) Uani 1 1 d . . . . .
C30 C 0.5768(3) 0.2766(8) 0.2353(4) 0.039(2) Uani 1 1 d . . . . .
C31 C 0.6226(4) 0.2983(10) 0.2857(4) 0.047(2) Uani 1 1 d . . . . .
H31A H 0.628903 0.224816 0.307551 0.071 Uiso 1 1 calc R U . . .
H31B H 0.612302 0.364206 0.306358 0.071 Uiso 1 1 calc R U . . .
H31C H 0.656254 0.319829 0.275684 0.071 Uiso 1 1 calc R U . . .
C32 C 0.5944(4) 0.1766(9) 0.2017(4) 0.050(2) Uani 1 1 d . . . . .
H32A H 0.627380 0.202184 0.191471 0.075 Uiso 1 1 calc R U . . .
H32B H 0.564701 0.161432 0.169283 0.075 Uiso 1 1 calc R U . . .
H32C H 0.602292 0.102549 0.223135 0.075 Uiso 1 1 calc R U . . .
C33 C 0.5246(4) 0.2402(10) 0.2497(5) 0.056(3) Uani 1 1 d . . . . .
H33A H 0.530013 0.161931 0.268049 0.084 Uiso 1 1 calc R U . . .
H33B H 0.494482 0.234055 0.216896 0.084 Uiso 1 1 calc R U . . .
H33C H 0.515492 0.300948 0.273616 0.084 Uiso 1 1 calc R U . . .
C34 C 0.5089(4) 0.5689(9) 0.1050(4) 0.055(2) Uani 1 1 d D U . . .
C35 C 0.5597(8) 0.548(2) 0.0882(9) 0.063(5) Uani 0.425(13) 1 d D U P B 1
H35A H 0.575315 0.469889 0.101747 0.095 Uiso 0.425(13) 1 calc R U P B 1
H35B H 0.586209 0.612096 0.102880 0.095 Uiso 0.425(13) 1 calc R U P B 1
H35C H 0.551274 0.548976 0.048856 0.095 Uiso 0.425(13) 1 calc R U P B 1
C36 C 0.4724(9) 0.4573(19) 0.0905(9) 0.068(6) Uani 0.425(13) 1 d D U P B 1
H36A H 0.455240 0.456368 0.051633 0.101 Uiso 0.425(13) 1 calc R U P B 1
H36B H 0.443744 0.459407 0.109793 0.101 Uiso 0.425(13) 1 calc R U P B 1
H36C H 0.494687 0.384507 0.100636 0.101 Uiso 0.425(13) 1 calc R U P B 1
C37 C 0.4774(10) 0.675(2) 0.0791(10) 0.067(6) Uani 0.425(13) 1 d D U P B 1
H37A H 0.498022 0.748475 0.092116 0.101 Uiso 0.425(13) 1 calc R U P B 1
H37B H 0.441944 0.677281 0.087949 0.101 Uiso 0.425(13) 1 calc R U P B 1
H37C H 0.471191 0.669026 0.040002 0.101 Uiso 0.425(13) 1 calc R U P B 1
C38 C 0.5473(8) 0.6687(18) 0.0957(8) 0.082(5) Uani 0.575(13) 1 d D U P B 2
H38A H 0.585441 0.645512 0.112152 0.123 Uiso 0.575(13) 1 calc R U P B 2
H38B H 0.539045 0.743848 0.112029 0.123 Uiso 0.575(13) 1 calc R U P B 2
H38C H 0.541893 0.680749 0.056988 0.123 Uiso 0.575(13) 1 calc R U P B 2
C39 C 0.5261(8) 0.4543(16) 0.0852(7) 0.072(5) Uani 0.575(13) 1 d D U P B 2
H39A H 0.515406 0.454213 0.045777 0.107 Uiso 0.575(13) 1 calc R U P B 2
H39B H 0.508179 0.386849 0.098397 0.107 Uiso 0.575(13) 1 calc R U P B 2
H39C H 0.565980 0.445782 0.098263 0.107 Uiso 0.575(13) 1 calc R U P B 2
C40 C 0.4523(6) 0.6031(19) 0.0756(7) 0.065(5) Uani 0.575(13) 1 d D U P B 2
H40A H 0.449644 0.608430 0.037044 0.097 Uiso 0.575(13) 1 calc R U P B 2
H40B H 0.443209 0.681400 0.088605 0.097 Uiso 0.575(13) 1 calc R U P B 2
H40C H 0.426531 0.542002 0.081690 0.097 Uiso 0.575(13) 1 calc R U P B 2
C41 C 0.4685(3) 0.9154(8) 0.2162(3) 0.0340(19) Uani 1 1 d . . . . .
C42 C 0.4685(3) 0.9489(9) 0.1642(3) 0.042(2) Uani 1 1 d . . . . .
H42 H 0.502793 0.958115 0.155978 0.051 Uiso 1 1 calc R U . . .
C43 C 0.4215(4) 0.9693(10) 0.1241(4) 0.051(3) Uani 1 1 d . . . . .
H43 H 0.423284 0.992408 0.089083 0.062 Uiso 1 1 calc R U . . .
C44 C 0.3717(4) 0.9557(10) 0.1356(4) 0.054(3) Uani 1 1 d . . . . .
H44 H 0.338557 0.967967 0.108335 0.065 Uiso 1 1 calc R U . . .
C45 C 0.3699(4) 0.9245(10) 0.1866(4) 0.046(2) Uani 1 1 d . . . . .
H45 H 0.335082 0.917014 0.193836 0.055 Uiso 1 1 calc R U . . .
C46 C 0.4174(3) 0.9027(8) 0.2289(3) 0.0342(19) Uani 1 1 d . . . . .
C47 C 0.3120(3) 0.7040(10) 0.2938(4) 0.045(2) Uani 1 1 d . . . . .
C48 C 0.3281(5) 0.5804(10) 0.2810(5) 0.065(3) Uani 1 1 d . . . . .
H48A H 0.303454 0.521050 0.290434 0.097 Uiso 1 1 calc R U . . .
H48B H 0.365934 0.564020 0.301604 0.097 Uiso 1 1 calc R U . . .
H48C H 0.325562 0.574853 0.242442 0.097 Uiso 1 1 calc R U . . .
C49 C 0.2533(4) 0.7305(12) 0.2645(5) 0.065(3) Uani 1 1 d . . . . .
H49A H 0.249367 0.728966 0.225606 0.098 Uiso 1 1 calc R U . . .
H49B H 0.243126 0.810360 0.274924 0.098 Uiso 1 1 calc R U . . .
H49C H 0.229304 0.669439 0.273722 0.098 Uiso 1 1 calc R U . . .
C50 C 0.3201(4) 0.7179(10) 0.3547(4) 0.053(3) Uani 1 1 d . . . . .
H50A H 0.295706 0.662039 0.366730 0.079 Uiso 1 1 calc R U . . .
H50B H 0.311568 0.800787 0.362811 0.079 Uiso 1 1 calc R U . . .
H50C H 0.358341 0.699565 0.373483 0.079 Uiso 1 1 calc R U . . .
C51 C 0.3985(3) 1.0471(9) 0.3503(4) 0.041(2) Uani 1 1 d . . . . .
C52 C 0.4037(4) 1.1314(10) 0.3054(5) 0.057(3) Uani 1 1 d . . . . .
H52A H 0.441787 1.131927 0.303077 0.086 Uiso 1 1 calc R U . . .
H52B H 0.392978 1.213082 0.312994 0.086 Uiso 1 1 calc R U . . .
H52C H 0.379619 1.103492 0.271196 0.086 Uiso 1 1 calc R U . . .
C53 C 0.3388(4) 1.0411(10) 0.3517(5) 0.056(3) Uani 1 1 d . . . . .
H53A H 0.317437 0.997788 0.319912 0.084 Uiso 1 1 calc R U . . .
H53B H 0.324306 1.123048 0.351793 0.084 Uiso 1 1 calc R U . . .
H53C H 0.336110 0.998684 0.384257 0.084 Uiso 1 1 calc R U . . .
C54 C 0.4341(4) 1.0913(11) 0.4045(5) 0.061(3) Uani 1 1 d . . . . .
H54A H 0.431867 1.033656 0.432700 0.092 Uiso 1 1 calc R U . . .
H54B H 0.420854 1.170224 0.412781 0.092 Uiso 1 1 calc R U . . .
H54C H 0.472235 1.098351 0.402811 0.092 Uiso 1 1 calc R U . . .
C55 C 0.4856(4) 0.6969(10) 0.4422(4) 0.047(2) Uani 1 1 d . . . . .
H55A H 0.486966 0.663185 0.478121 0.057 Uiso 1 1 calc R U . . .
H55B H 0.446599 0.708741 0.422615 0.057 Uiso 1 1 calc R U . . .
C56 C 0.5151(4) 0.8148(10) 0.4483(4) 0.052(3) Uani 1 1 d . . . . .
H56A H 0.512739 0.848848 0.412655 0.078 Uiso 1 1 calc R U . . .
H56B H 0.553711 0.802501 0.467456 0.078 Uiso 1 1 calc R U . . .
H56C H 0.498206 0.870591 0.468737 0.078 Uiso 1 1 calc R U . . .
C57 C 0.4863(4) 0.4977(11) 0.4066(4) 0.057(3) Uani 1 1 d . . . . .
H57A H 0.448035 0.503470 0.384087 0.068 Uiso 1 1 calc R U . . .
H57B H 0.485528 0.465255 0.442220 0.068 Uiso 1 1 calc R U . . .
C58 C 0.5184(5) 0.4156(10) 0.3807(5) 0.065(3) Uani 1 1 d . . . . .
H58A H 0.516613 0.444716 0.344390 0.097 Uiso 1 1 calc R U . . .
H58B H 0.503021 0.334126 0.378631 0.097 Uiso 1 1 calc R U . . .
H58C H 0.556752 0.414033 0.402078 0.097 Uiso 1 1 calc R U . . .
C59 C 0.7459(5) 0.2594(12) 0.4137(5) 0.066(3) Uani 1 1 d . . . . .
H59A H 0.743177 0.186770 0.390840 0.079 Uiso 1 1 calc R U . . .
H59B H 0.708185 0.282673 0.414052 0.079 Uiso 1 1 calc R U . . .
C60 C 0.7765(5) 0.2277(12) 0.4688(5) 0.075(4) Uani 1 1 d . . . . .
H60A H 0.811291 0.189300 0.468116 0.112 Uiso 1 1 calc R U . . .
H60B H 0.754700 0.171718 0.484121 0.112 Uiso 1 1 calc R U . . .
H60C H 0.783977 0.300835 0.490809 0.112 Uiso 1 1 calc R U . . .
C61 C 0.8175(4) 0.3208(10) 0.3760(5) 0.057(3) Uani 1 1 d . . . . .
H61A H 0.810407 0.248205 0.352867 0.069 Uiso 1 1 calc R U . . .
H61B H 0.846245 0.300679 0.409130 0.069 Uiso 1 1 calc R U . . .
C62 C 0.8373(5) 0.4217(12) 0.3468(5) 0.072(4) Uani 1 1 d . . . . .
H62A H 0.807794 0.445729 0.315458 0.108 Uiso 1 1 calc R U . . .
H62B H 0.869046 0.394322 0.334792 0.108 Uiso 1 1 calc R U . . .
H62C H 0.847915 0.490764 0.370979 0.108 Uiso 1 1 calc R U . . .
C63 C 0.3038(4) 0.5022(12) 0.1177(6) 0.083(4) Uani 1 1 d D . . . .
H63A H 0.273091 0.469407 0.130706 0.099 Uiso 1 1 calc R U . . .
H63B H 0.300626 0.469726 0.081251 0.099 Uiso 1 1 calc R U . . .
C64 C 0.3007(5) 0.6309(12) 0.1157(5) 0.077(4) Uani 1 1 d D . . . .
H64A H 0.266327 0.655664 0.090264 0.115 Uiso 1 1 calc R U . . .
H64B H 0.331839 0.662990 0.104042 0.115 Uiso 1 1 calc R U . . .
H64C H 0.301863 0.662327 0.151566 0.115 Uiso 1 1 calc R U . . .
C65 C 0.3507(10) 0.3375(15) 0.1455(11) 0.085(4) Uani 0.586(19) 1 d D U P C 1
H65A H 0.315157 0.307103 0.149532 0.102 Uiso 0.586(19) 1 calc R U P C 1
H65B H 0.354487 0.314783 0.109536 0.102 Uiso 0.586(19) 1 calc R U P C 1
C66 C 0.3956(11) 0.290(3) 0.1872(11) 0.111(7) Uani 0.586(19) 1 d D U P C 1
H66A H 0.429465 0.294059 0.175507 0.166 Uiso 0.586(19) 1 calc R U P C 1
H66B H 0.387936 0.206253 0.194563 0.166 Uiso 0.586(19) 1 calc R U P C 1
H66C H 0.399963 0.338215 0.220024 0.166 Uiso 0.586(19) 1 calc R U P C 1
C67 C 0.3678(16) 0.355(2) 0.1810(12) 0.088(5) Uani 0.414(19) 1 d D U P C 2
H67A H 0.338603 0.331628 0.198307 0.105 Uiso 0.414(19) 1 calc R U P C 2
H67B H 0.402961 0.361356 0.209113 0.105 Uiso 0.414(19) 1 calc R U P C 2
C68 C 0.3720(17) 0.268(3) 0.1409(15) 0.109(7) Uani 0.414(19) 1 d D U P C 2
H68A H 0.397089 0.297885 0.120689 0.163 Uiso 0.414(19) 1 calc R U P C 2
H68B H 0.335653 0.254373 0.116309 0.163 Uiso 0.414(19) 1 calc R U P C 2
H68C H 0.386069 0.191601 0.158522 0.163 Uiso 0.414(19) 1 calc R U P C 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'
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 0 -1 0.0264
-1 0 1 0.0196
0 -2 -1 0.1582
-1 -2 0 0.1513
0 2 1 0.1267
1 2 0 0.1229
2 0 -1 0.0232
1 0 0 0.0243
1 0 1 0.0344
0 -3 15 0.0612
-1 0 -2 0.0120
-2 1 -1 0.0858
-13 1 -6 0.0295
-16 -2 5 0.0519
0 5 12 0.1007
9 -3 9 0.0750
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
K2 Ce1 K1 117.25(4) . . ?
O1 Ce1 K1 38.92(14) . . ?
O1 Ce1 K2 151.93(15) . . ?
O1 Ce1 O10 77.32(18) . . ?
O1 Ce1 C1 80.6(2) . . ?
O1 Ce1 C2 70.8(2) . . ?
O1 Ce1 C3 85.89(19) . . ?
O1 Ce1 C4 115.74(19) . . ?
O1 Ce1 C5 129.7(2) . . ?
O1 Ce1 C6 111.2(2) . . ?
O4 Ce1 K1 71.76(13) . . ?
O4 Ce1 K2 46.29(13) . . ?
O4 Ce1 O1 106.3(2) . . ?
O4 Ce1 O7 88.44(18) . . ?
O4 Ce1 O10 108.69(19) . . ?
O4 Ce1 C1 129.6(2) . . ?
O4 Ce1 C2 105.6(2) . . ?
O4 Ce1 C3 77.7(2) . . ?
O4 Ce1 C4 72.4(2) . . ?
O4 Ce1 C5 92.7(2) . . ?
O4 Ce1 C6 123.4(2) . . ?
O7 Ce1 K1 157.97(14) . . ?
O7 Ce1 K2 46.01(13) . . ?
O7 Ce1 O1 148.74(18) . . ?
O7 Ce1 O10 71.83(17) . . ?
O7 Ce1 C1 111.4(2) . . ?
O7 Ce1 C2 132.4(2) . . ?
O7 Ce1 C3 124.67(19) . . ?
O7 Ce1 C4 94.80(19) . . ?
O7 Ce1 C5 75.3(2) . . ?
O7 Ce1 C6 80.8(2) . . ?
O10 Ce1 K1 104.85(13) . . ?
O10 Ce1 K2 103.47(13) . . ?
O10 Ce1 C1 121.4(2) . . ?
O10 Ce1 C2 138.3(2) . . ?
O10 Ce1 C3 163.09(18) . . ?
O10 Ce1 C4 166.41(19) . . ?
O10 Ce1 C5 139.8(2) . . ?
C1 Ce1 K1 89.20(17) . . ?
C1 Ce1 K2 119.92(16) . . ?
C1 Ce1 C2 28.3(2) . . ?
C1 Ce1 C3 52.6(2) . . ?
C1 Ce1 C4 60.5(2) . . ?
C1 Ce1 C5 52.7(2) . . ?
C2 Ce1 K1 64.62(16) . . ?
C2 Ce1 K2 117.32(15) . . ?
C3 Ce1 K1 61.54(15) . . ?
C3 Ce1 K2 92.26(14) . . ?
C3 Ce1 C2 28.9(2) . . ?
C3 Ce1 C4 29.9(2) . . ?
C3 Ce1 C5 52.7(2) . . ?
C4 Ce1 K1 88.44(16) . . ?
C4 Ce1 K2 67.07(15) . . ?
C4 Ce1 C2 50.3(2) . . ?
C5 Ce1 K1 114.21(17) . . ?
C5 Ce1 K2 67.19(17) . . ?
C5 Ce1 C2 59.2(2) . . ?
C5 Ce1 C4 28.5(2) . . ?
C6 Ce1 K1 117.91(17) . . ?
C6 Ce1 K2 93.07(17) . . ?
C6 Ce1 O10 119.6(2) . . ?
C6 Ce1 C1 31.6(2) . . ?
C6 Ce1 C2 53.3(2) . . ?
C6 Ce1 C3 64.7(2) . . ?
C6 Ce1 C4 53.7(2) . . ?
C6 Ce1 C5 30.9(2) . . ?
Si1 K1 Ce1 55.78(4) . . ?
Si1 K1 C28 134.06(17) . . ?
O1 K1 Ce1 32.67(11) . . ?
O1 K1 Si1 27.30(12) . . ?
O1 K1 O3 55.66(16) . . ?
O1 K1 C24 84.60(19) . . ?
O1 K1 C25 99.0(2) . . ?
O1 K1 C26 124.0(2) . . ?
O1 K1 C28 120.90(19) . . ?
O1 K1 C29 97.46(19) . . ?
O3 K1 Ce1 79.78(11) . . ?
O3 K1 Si1 28.68(12) . . ?
O3 K1 C24 92.3(2) . . ?
O3 K1 C25 81.4(2) . . ?
O3 K1 C26 95.8(2) . . ?
O3 K1 C28 130.6(2) . . ?
O3 K1 C29 118.4(2) . . ?
O11 K1 Ce1 147.44(17) . . ?
O11 K1 Si1 117.34(17) . . ?
O11 K1 O1 126.4(2) . . ?
O11 K1 O3 106.8(2) . . ?
O11 K1 C24 148.9(2) . . ?
O11 K1 C25 130.5(2) . . ?
O11 K1 C26 106.5(2) . . ?
O11 K1 C28 108.2(2) . . ?
O11 K1 C29 130.0(2) . . ?
C24 K1 Ce1 58.83(14) . . ?
C24 K1 Si1 91.20(17) . . ?
C24 K1 C26 45.8(2) . . ?
C24 K1 C28 43.0(2) . . ?
C24 K1 C29 26.2(2) . . ?
C25 K1 Ce1 81.71(17) . . ?
C25 K1 Si1 93.38(19) . . ?
C25 K1 C24 27.5(2) . . ?
C25 K1 C26 25.0(2) . . ?
C25 K1 C28 49.3(2) . . ?
C25 K1 C29 45.9(2) . . ?
C26 K1 Ce1 104.36(16) . . ?
C26 K1 Si1 114.9(2) . . ?
C26 K1 C28 41.0(2) . . ?
C26 K1 C29 51.2(2) . . ?
C28 K1 Ce1 88.74(14) . . ?
C29 K1 Ce1 65.59(15) . . ?
C29 K1 Si1 112.56(17) . . ?
C29 K1 C28 23.5(2) . . ?
Si2 K2 Ce1 61.66(5) . . ?
Si2 K2 C41 93.66(16) . . ?
Si3 K2 Ce1 60.99(5) . . ?
Si3 K2 Si2 121.28(8) . . ?
Si3 K2 C41 51.46(15) . . ?
O4 K2 Ce1 38.21(12) . . ?
O4 K2 Si2 27.99(12) . . ?
O4 K2 Si3 98.94(13) . . ?
O4 K2 C41 91.89(19) . . ?
O4 K2 C46 108.72(19) . . ?
O6 K2 Ce1 85.62(12) . . ?
O6 K2 Si2 29.00(13) . . ?
O6 K2 Si3 135.66(15) . . ?
O6 K2 O4 56.75(17) . . ?
O6 K2 O7 123.49(17) . . ?
O6 K2 O12 100.3(2) . . ?
O6 K2 C41 89.7(2) . . ?
O6 K2 C46 114.0(2) . . ?
O7 K2 Ce1 38.31(10) . . ?
O7 K2 Si2 99.58(12) . . ?
O7 K2 Si3 28.06(12) . . ?
O7 K2 O4 73.57(16) . . ?
O7 K2 C41 65.14(19) . . ?
O7 K2 C46 56.5(2) . . ?
O12 K2 Ce1 151.2(2) . . ?
O12 K2 Si2 112.84(19) . . ?
O12 K2 Si3 123.21(19) . . ?
O12 K2 O4 124.5(2) . . ?
O12 K2 O7 131.3(2) . . ?
O12 K2 C41 141.7(2) . . ?
O12 K2 C46 126.5(2) . . ?
C41 K2 Ce1 65.63(14) . . ?
C46 K2 Ce1 74.18(15) . . ?
C46 K2 Si2 117.05(16) . . ?
C46 K2 Si3 33.26(16) . . ?
C46 K2 C41 24.7(2) . . ?
O1 Si1 K1 52.5(2) . . ?
O1 Si1 O2 113.2(3) . . ?
O1 Si1 O3 105.0(3) . . ?
O1 Si1 C12 115.8(3) . . ?
O2 Si1 K1 117.9(3) . . ?
O2 Si1 O3 108.3(3) . . ?
O2 Si1 C12 102.4(3) . . ?
O3 Si1 K1 53.3(2) . . ?
O3 Si1 C12 112.2(3) . . ?
C12 Si1 K1 139.5(2) . . ?
O4 Si2 K2 53.9(2) . . ?
O4 Si2 O5 114.3(3) . . ?
O4 Si2 O6 104.9(3) . . ?
O4 Si2 C29 112.4(3) . . ?
O5 Si2 K2 114.5(2) . . ?
O5 Si2 O6 102.6(3) . . ?
O5 Si2 C29 107.5(4) . . ?
O6 Si2 K2 51.6(2) . . ?
O6 Si2 C29 114.9(4) . . ?
C29 Si2 K2 137.7(3) . . ?
O7 Si3 K2 53.6(2) . . ?
O7 Si3 O8 112.7(3) . . ?
O7 Si3 O9 111.3(3) . . ?
O7 Si3 C46 109.1(3) . . ?
O8 Si3 K2 87.2(3) . . ?
O8 Si3 C46 101.0(3) . . ?
O9 Si3 K2 162.3(2) . . ?
O9 Si3 O8 108.9(3) . . ?
O9 Si3 C46 113.5(4) . . ?
C46 Si3 K2 68.9(3) . . ?
Ce1 O1 K1 108.4(2) . . ?
Si1 O1 Ce1 130.1(3) . . ?
Si1 O1 K1 100.2(3) . . ?
C13 O2 Si1 132.0(6) . . ?
Si1 O3 K1 98.1(3) . . ?
C17 O3 K1 125.1(5) . . ?
C17 O3 Si1 133.9(5) . . ?
Ce1 O4 K2 95.50(19) . . ?
Si2 O4 Ce1 136.9(3) . . ?
Si2 O4 K2 98.1(3) . . ?
C30 O5 Si2 132.9(6) . . ?
Si2 O6 K2 99.4(3) . . ?
C34 O6 K2 126.3(5) . . ?
C34 O6 Si2 133.0(5) . . ?
Ce1 O7 K2 95.69(17) . . ?
Si3 O7 Ce1 133.3(3) . . ?
Si3 O7 K2 98.3(2) . . ?
C47 O8 Si3 134.3(5) . . ?
C51 O9 Si3 136.3(6) . . ?
C55 O10 Ce1 117.8(5) . . ?
C57 O10 Ce1 118.1(5) . . ?
C57 O10 C55 113.0(7) . . ?
C59 O11 K1 115.9(6) . . ?
C61 O11 K1 127.9(6) . . ?
C61 O11 C59 112.9(9) . . ?
C63 O12 K2 124.9(7) . . ?
C63 O12 C65 99.9(12) . . ?
C63 O12 C67 127.9(18) . . ?
C65 O12 K2 135.0(10) . . ?
C67 O12 K2 103.9(16) . . ?
C2 C1 Ce1 81.7(5) . . ?
C2 C1 C6 121.3(7) . . ?
C2 C1 C7 119.9(7) . . ?
C6 C1 Ce1 69.5(4) . . ?
C6 C1 C7 118.7(7) . . ?
C7 C1 Ce1 115.9(5) . . ?
Ce1 C2 H2 118.1 . . ?
C1 C2 Ce1 70.0(4) . . ?
C1 C2 H2 118.1 . . ?
C1 C2 C3 121.9(7) . . ?
C3 C2 Ce1 71.9(4) . . ?
C3 C2 H2 118.1 . . ?
C2 C3 Ce1 79.3(4) . . ?
C2 C3 C4 115.5(7) . . ?
C2 C3 C24 122.1(7) . . ?
C4 C3 Ce1 76.3(4) . . ?
C24 C3 Ce1 117.8(5) . . ?
C24 C3 C4 122.1(7) . . ?
Ce1 C4 H4 118.7 . . ?
C3 C4 Ce1 73.8(4) . . ?
C3 C4 H4 118.7 . . ?
C5 C4 Ce1 75.3(5) . . ?
C5 C4 C3 122.3(7) . . ?
C5 C4 H4 118.7 . . ?
C4 C5 Ce1 76.1(5) . . ?
C4 C5 C6 120.0(7) . . ?
C4 C5 C41 117.0(7) . . ?
C6 C5 Ce1 67.0(4) . . ?
C6 C5 C41 123.0(8) . . ?
C41 C5 Ce1 126.7(5) . . ?
Ce1 C6 H6 121.3 . . ?
C1 C6 Ce1 78.9(5) . . ?
C1 C6 H6 121.3 . . ?
C5 C6 Ce1 82.1(5) . . ?
C5 C6 C1 115.4(7) . . ?
C5 C6 H6 121.3 . . ?
C8 C7 C1 117.5(7) . . ?
C8 C7 C12 120.3(8) . . ?
C12 C7 C1 122.0(8) . . ?
C7 C8 H8 119.3 . . ?
C7 C8 C9 121.5(9) . . ?
C9 C8 H8 119.3 . . ?
C8 C9 H9 119.8 . . ?
C10 C9 C8 120.4(9) . . ?
C10 C9 H9 119.8 . . ?
C9 C10 H10 121.2 . . ?
C9 C10 C11 117.6(9) . . ?
C11 C10 H10 121.2 . . ?
C10 C11 H11 117.9 . . ?
C12 C11 C10 124.2(9) . . ?
C12 C11 H11 117.9 . . ?
C7 C12 Si1 127.2(6) . . ?
C11 C12 Si1 116.4(7) . . ?
C11 C12 C7 116.1(8) . . ?
O2 C13 C14 108.1(7) . . ?
O2 C13 C15 106.1(8) . . ?
O2 C13 C16 111.9(8) . . ?
C15 C13 C14 108.2(8) . . ?
C16 C13 C14 110.2(9) . . ?
C16 C13 C15 112.2(8) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O3 C17 C18 112.1(8) . . ?
O3 C17 C19 107.9(7) . . ?
O3 C17 C20 106.3(7) . . ?
O3 C17 C21 99(2) . . ?
O3 C17 C22 113(2) . . ?
O3 C17 C23 111(2) . . ?
C18 C17 C19 111.1(8) . . ?
C18 C17 C20 111.0(8) . . ?
C20 C17 C19 108.2(7) . . ?
C22 C17 C21 109.0(15) . . ?
C23 C17 C21 111.0(15) . . ?
C23 C17 C22 112.2(15) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C17 C21 H21A 109.5 . . ?
C17 C21 H21B 109.5 . . ?
C17 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C17 C22 H22A 109.5 . . ?
C17 C22 H22B 109.5 . . ?
C17 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C17 C23 H23A 109.5 . . ?
C17 C23 H23B 109.5 . . ?
C17 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C3 C24 K1 107.8(5) . . ?
C3 C24 C25 118.4(8) . . ?
C3 C24 C29 125.4(7) . . ?
C25 C24 K1 73.6(5) . . ?
C25 C24 C29 116.2(7) . . ?
C29 C24 K1 84.6(5) . . ?
K1 C25 H25 103.3 . . ?
C24 C25 K1 78.9(5) . . ?
C24 C25 H25 118.9 . . ?
C26 C25 K1 88.3(6) . . ?
C26 C25 C24 122.2(8) . . ?
C26 C25 H25 118.9 . . ?
K1 C26 H26 114.2 . . ?
C25 C26 K1 66.6(5) . . ?
C25 C26 H26 119.3 . . ?
C25 C26 C27 121.3(8) . . ?
C27 C26 K1 89.7(6) . . ?
C27 C26 H26 119.3 . . ?
C26 C27 H27 121.4 . . ?
C28 C27 C26 117.1(9) . . ?
C28 C27 H27 121.4 . . ?
K1 C28 H28 125.2 . . ?
C27 C28 K1 80.1(6) . . ?
C27 C28 H28 117.7 . . ?
C27 C28 C29 124.6(9) . . ?
C29 C28 K1 68.6(5) . . ?
C29 C28 H28 117.7 . . ?
Si2 C29 K1 106.3(3) . . ?
C24 C29 K1 69.1(5) . . ?
C24 C29 Si2 124.0(6) . . ?
C28 C29 K1 87.9(5) . . ?
C28 C29 Si2 117.2(7) . . ?
C28 C29 C24 118.3(7) . . ?
O5 C30 C31 111.4(7) . . ?
O5 C30 C32 106.6(7) . . ?
O5 C30 C33 109.1(8) . . ?
C31 C30 C32 109.1(8) . . ?
C31 C30 C33 110.4(8) . . ?
C33 C30 C32 110.1(8) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O6 C34 C35 117.0(11) . . ?
O6 C34 C36 99.6(11) . . ?
O6 C34 C37 108.8(12) . . ?
O6 C34 C38 104.0(10) . . ?
O6 C34 C39 115.5(10) . . ?
O6 C34 C40 109.0(10) . . ?
C35 C34 C36 108.5(11) . . ?
C35 C34 C37 113.5(11) . . ?
C37 C34 C36 108.3(11) . . ?
C39 C34 C38 108.2(10) . . ?
C39 C34 C40 112.1(10) . . ?
C40 C34 C38 107.5(10) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C34 C38 H38A 109.5 . . ?
C34 C38 H38B 109.5 . . ?
C34 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C34 C39 H39A 109.5 . . ?
C34 C39 H39B 109.5 . . ?
C34 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C34 C40 H40A 109.5 . . ?
C34 C40 H40B 109.5 . . ?
C34 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C5 C41 K2 92.2(5) . . ?
C42 C41 K2 105.5(6) . . ?
C42 C41 C5 117.3(8) . . ?
C42 C41 C46 118.6(8) . . ?
C46 C41 K2 71.1(5) . . ?
C46 C41 C5 124.0(7) . . ?
C41 C42 H42 118.3 . . ?
C43 C42 C41 123.4(9) . . ?
C43 C42 H42 118.3 . . ?
C42 C43 H43 120.7 . . ?
C42 C43 C44 118.6(9) . . ?
C44 C43 H43 120.7 . . ?
C43 C44 H44 120.1 . . ?
C45 C44 C43 119.8(8) . . ?
C45 C44 H44 120.1 . . ?
C44 C45 H45 118.4 . . ?
C44 C45 C46 123.2(9) . . ?
C46 C45 H45 118.4 . . ?
Si3 C46 K2 77.8(3) . . ?
C41 C46 K2 84.2(5) . . ?
C41 C46 Si3 124.0(6) . . ?
C45 C46 K2 98.9(6) . . ?
C45 C46 Si3 118.6(7) . . ?
C45 C46 C41 116.4(8) . . ?
O8 C47 C48 108.9(8) . . ?
O8 C47 C49 105.5(8) . . ?
O8 C47 C50 110.9(8) . . ?
C48 C47 C49 110.9(9) . . ?
C48 C47 C50 110.3(9) . . ?
C49 C47 C50 110.1(8) . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C47 C50 H50A 109.5 . . ?
C47 C50 H50B 109.5 . . ?
C47 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
O9 C51 C52 111.2(7) . . ?
O9 C51 C53 109.5(8) . . ?
O9 C51 C54 106.4(8) . . ?
C52 C51 C54 110.5(9) . . ?
C53 C51 C52 109.2(8) . . ?
C53 C51 C54 109.9(8) . . ?
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 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
O10 C55 H55A 109.8 . . ?
O10 C55 H55B 109.8 . . ?
O10 C55 C56 109.4(7) . . ?
H55A C55 H55B 108.2 . . ?
C56 C55 H55A 109.8 . . ?
C56 C55 H55B 109.8 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
O10 C57 H57A 109.8 . . ?
O10 C57 H57B 109.8 . . ?
O10 C57 C58 109.2(8) . . ?
H57A C57 H57B 108.3 . . ?
C58 C57 H57A 109.8 . . ?
C58 C57 H57B 109.8 . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
O11 C59 H59A 108.4 . . ?
O11 C59 H59B 108.4 . . ?
O11 C59 C60 115.4(10) . . ?
H59A C59 H59B 107.5 . . ?
C60 C59 H59A 108.4 . . ?
C60 C59 H59B 108.4 . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
O11 C61 H61A 109.6 . . ?
O11 C61 H61B 109.6 . . ?
O11 C61 C62 110.3(9) . . ?
H61A C61 H61B 108.1 . . ?
C62 C61 H61A 109.6 . . ?
C62 C61 H61B 109.6 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62B 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
O12 C63 H63A 109.8 . . ?
O12 C63 H63B 109.8 . . ?
O12 C63 C64 109.3(9) . . ?
H63A C63 H63B 108.3 . . ?
C64 C63 H63A 109.8 . . ?
C64 C63 H63B 109.8 . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
O12 C65 H65A 110.8 . . ?
O12 C65 H65B 110.8 . . ?
H65A C65 H65B 108.9 . . ?
C66 C65 O12 104.5(19) . . ?
C66 C65 H65A 110.8 . . ?
C66 C65 H65B 110.8 . . ?
C65 C66 H66A 109.5 . . ?
C65 C66 H66B 109.5 . . ?
C65 C66 H66C 109.5 . . ?
H66A C66 H66B 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
O12 C67 H67A 110.6 . . ?
O12 C67 H67B 110.6 . . ?
O12 C67 C68 106(2) . . ?
H67A C67 H67B 108.7 . . ?
C68 C67 H67A 110.6 . . ?
C68 C67 H67B 110.6 . . ?
C67 C68 H68A 109.5 . . ?
C67 C68 H68B 109.5 . . ?
C67 C68 H68C 109.5 . . ?
H68A C68 H68B 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
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 K1 4.1768(18) . ?
Ce1 K2 3.7873(18) . ?
Ce1 O1 2.376(5) . ?
Ce1 O4 2.353(5) . ?
Ce1 O7 2.359(5) . ?
Ce1 O10 2.682(6) . ?
Ce1 C1 2.745(8) . ?
Ce1 C2 2.892(7) . ?
Ce1 C3 2.797(7) . ?
Ce1 C4 2.830(8) . ?
Ce1 C5 2.820(8) . ?
Ce1 C6 2.621(8) . ?
K1 Si1 3.432(3) . ?
K1 O1 2.765(6) . ?
K1 O3 2.777(6) . ?
K1 O11 2.737(7) . ?
K1 C24 3.069(9) . ?
K1 C25 3.000(9) . ?
K1 C26 3.266(10) . ?
K1 C28 3.510(9) . ?
K1 C29 3.270(8) . ?
K2 Si2 3.371(3) . ?
K2 Si3 3.365(3) . ?
K2 O4 2.750(6) . ?
K2 O6 2.679(6) . ?
K2 O7 2.738(6) . ?
K2 O12 2.720(9) . ?
K2 C41 3.378(9) . ?
K2 C46 3.212(9) . ?
Si1 O1 1.599(6) . ?
Si1 O2 1.638(6) . ?
Si1 O3 1.663(6) . ?
Si1 C12 1.908(9) . ?
Si2 O4 1.598(6) . ?
Si2 O5 1.636(7) . ?
Si2 O6 1.656(6) . ?
Si2 C29 1.872(8) . ?
Si3 O7 1.600(6) . ?
Si3 O8 1.651(6) . ?
Si3 O9 1.627(7) . ?
Si3 C46 1.888(9) . ?
O2 C13 1.428(11) . ?
O3 C17 1.456(9) . ?
O5 C30 1.443(11) . ?
O6 C34 1.428(11) . ?
O8 C47 1.432(11) . ?
O9 C51 1.448(11) . ?
O10 C55 1.444(11) . ?
O10 C57 1.427(13) . ?
O11 C59 1.432(13) . ?
O11 C61 1.408(12) . ?
O12 C63 1.418(13) . ?
O12 C65 1.446(16) . ?
O12 C67 1.432(18) . ?
C1 C2 1.386(12) . ?
C1 C6 1.465(10) . ?
C1 C7 1.517(11) . ?
C2 H2 1.0000 . ?
C2 C3 1.422(11) . ?
C3 C4 1.453(10) . ?
C3 C24 1.427(11) . ?
C4 H4 1.0000 . ?
C4 C5 1.393(12) . ?
C5 C6 1.461(12) . ?
C5 C41 1.490(11) . ?
C6 H6 1.0000 . ?
C7 C8 1.378(12) . ?
C7 C12 1.411(11) . ?
C8 H8 0.9500 . ?
C8 C9 1.381(12) . ?
C9 H9 0.9500 . ?
C9 C10 1.370(13) . ?
C10 H10 0.9500 . ?
C10 C11 1.398(14) . ?
C11 H11 0.9500 . ?
C11 C12 1.386(12) . ?
C13 C14 1.540(11) . ?
C13 C15 1.516(13) . ?
C13 C16 1.477(14) . ?
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 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.492(12) . ?
C17 C19 1.522(11) . ?
C17 C20 1.520(11) . ?
C17 C21 1.527(17) . ?
C17 C22 1.508(17) . ?
C17 C23 1.490(17) . ?
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 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.442(11) . ?
C24 C29 1.451(13) . ?
C25 H25 0.9500 . ?
C25 C26 1.383(13) . ?
C26 H26 0.9500 . ?
C26 C27 1.402(14) . ?
C27 H27 0.9500 . ?
C27 C28 1.390(12) . ?
C28 H28 0.9500 . ?
C28 C29 1.399(12) . ?
C30 C31 1.513(12) . ?
C30 C32 1.542(13) . ?
C30 C33 1.517(12) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.476(15) . ?
C34 C36 1.531(15) . ?
C34 C37 1.477(15) . ?
C34 C38 1.532(14) . ?
C34 C39 1.477(14) . ?
C34 C40 1.480(13) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C42 1.390(12) . ?
C41 C46 1.418(11) . ?
C42 H42 0.9500 . ?
C42 C43 1.373(12) . ?
C43 H43 0.9500 . ?
C43 C44 1.374(14) . ?
C44 H44 0.9500 . ?
C44 C45 1.370(13) . ?
C45 H45 0.9500 . ?
C45 C46 1.413(12) . ?
C47 C48 1.493(15) . ?
C47 C49 1.505(13) . ?
C47 C50 1.535(13) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 C52 1.521(14) . ?
C51 C53 1.518(13) . ?
C51 C54 1.529(14) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C55 C56 1.494(14) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C57 C58 1.489(16) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C59 C60 1.469(16) . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C61 C62 1.506(16) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C63 C64 1.431(15) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C65 C66 1.440(19) . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C67 C68 1.44(2) . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
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
Ce1 O10 C55 C56 -38.4(8) . . . . ?
Ce1 O10 C57 C58 42.1(9) . . . . ?
Ce1 C1 C2 C3 51.9(7) . . . . ?
Ce1 C1 C6 C5 -75.7(6) . . . . ?
Ce1 C1 C7 C8 -124.5(7) . . . . ?
Ce1 C1 C7 C12 50.6(9) . . . . ?
Ce1 C2 C3 C4 69.0(6) . . . . ?
Ce1 C2 C3 C24 -116.2(8) . . . . ?
Ce1 C3 C4 C5 60.3(7) . . . . ?
Ce1 C3 C24 K1 -42.2(6) . . . . ?
Ce1 C3 C24 C25 -122.8(7) . . . . ?
Ce1 C3 C24 C29 54.0(10) . . . . ?
Ce1 C4 C5 C6 52.6(7) . . . . ?
Ce1 C4 C5 C41 -124.4(7) . . . . ?
Ce1 C5 C6 C1 73.7(6) . . . . ?
Ce1 C5 C41 K2 -31.0(7) . . . . ?
Ce1 C5 C41 C42 -139.7(7) . . . . ?
Ce1 C5 C41 C46 37.5(12) . . . . ?
K1 Si1 O1 Ce1 -124.9(4) . . . . ?
K1 Si1 O2 C13 -38.2(7) . . . . ?
K1 Si1 O3 C17 -160.4(8) . . . . ?
K1 O3 C17 C18 162.6(7) . . . . ?
K1 O3 C17 C19 -74.7(8) . . . . ?
K1 O3 C17 C20 41.2(9) . . . . ?
K1 O3 C17 C21 115.5(17) . . . . ?
K1 O3 C17 C22 -129.0(19) . . . . ?
K1 O3 C17 C23 -1.5(19) . . . . ?
K1 O11 C59 C60 -127.5(9) . . . . ?
K1 O11 C61 C62 17.4(13) . . . . ?
K1 C24 C25 C26 80.9(9) . . . . ?
K1 C24 C29 Si2 96.0(6) . . . . ?
K1 C24 C29 C28 -75.6(7) . . . . ?
K1 C25 C26 C27 74.4(9) . . . . ?
K1 C26 C27 C28 60.8(9) . . . . ?
K1 C28 C29 Si2 -107.2(6) . . . . ?
K1 C28 C29 C24 64.9(7) . . . . ?
K2 Si2 O4 Ce1 -107.1(5) . . . . ?
K2 Si2 O5 C30 -92.4(7) . . . . ?
K2 Si2 O6 C34 -166.9(9) . . . . ?
K2 Si2 C29 K1 103.8(4) . . . . ?
K2 Si2 C29 C24 28.3(10) . . . . ?
K2 Si2 C29 C28 -160.0(5) . . . . ?
K2 Si3 O7 Ce1 106.0(4) . . . . ?
K2 Si3 O8 C47 90.9(9) . . . . ?
K2 Si3 O9 C51 141.2(7) . . . . ?
K2 Si3 C46 C41 -74.3(8) . . . . ?
K2 Si3 C46 C45 93.5(8) . . . . ?
K2 O6 C34 C35 176.6(12) . . . . ?
K2 O6 C34 C36 -66.9(11) . . . . ?
K2 O6 C34 C37 46.3(13) . . . . ?
K2 O6 C34 C38 118.6(10) . . . . ?
K2 O6 C34 C39 -123.0(10) . . . . ?
K2 O6 C34 C40 4.2(12) . . . . ?
K2 O12 C63 C64 0.4(16) . . . . ?
K2 O12 C65 C66 15(3) . . . . ?
K2 O12 C67 C68 -126(3) . . . . ?
K2 C41 C42 C43 75.9(11) . . . . ?
K2 C41 C46 Si3 71.1(6) . . . . ?
K2 C41 C46 C45 -97.0(8) . . . . ?
Si1 O2 C13 C14 -76.2(10) . . . . ?
Si1 O2 C13 C15 167.9(7) . . . . ?
Si1 O2 C13 C16 45.3(10) . . . . ?
Si1 O3 C17 C18 -41.4(11) . . . . ?
Si1 O3 C17 C19 81.3(9) . . . . ?
Si1 O3 C17 C20 -162.8(7) . . . . ?
Si1 O3 C17 C21 -88.5(18) . . . . ?
Si1 O3 C17 C22 27(2) . . . . ?
Si1 O3 C17 C23 154.5(18) . . . . ?
Si2 O5 C30 C31 -43.0(10) . . . . ?
Si2 O5 C30 C32 -161.9(6) . . . . ?
Si2 O5 C30 C33 79.2(9) . . . . ?
Si2 O6 C34 C35 -19.5(15) . . . . ?
Si2 O6 C34 C36 97.0(12) . . . . ?
Si2 O6 C34 C37 -149.7(12) . . . . ?
Si2 O6 C34 C38 -77.5(11) . . . . ?
Si2 O6 C34 C39 40.9(13) . . . . ?
Si2 O6 C34 C40 168.1(10) . . . . ?
Si3 O8 C47 C48 -71.6(11) . . . . ?
Si3 O8 C47 C49 169.2(8) . . . . ?
Si3 O8 C47 C50 50.0(12) . . . . ?
Si3 O9 C51 C52 -46.5(11) . . . . ?
Si3 O9 C51 C53 74.3(11) . . . . ?
Si3 O9 C51 C54 -166.9(7) . . . . ?
O1 Si1 O2 C13 20.3(8) . . . . ?
O1 Si1 O3 K1 -9.5(3) . . . . ?
O1 Si1 O3 C17 -169.9(7) . . . . ?
O2 Si1 O1 Ce1 126.9(4) . . . . ?
O2 Si1 O1 K1 -108.3(3) . . . . ?
O2 Si1 O3 K1 111.7(3) . . . . ?
O2 Si1 O3 C17 -48.7(8) . . . . ?
O3 Si1 O1 Ce1 -115.3(4) . . . . ?
O3 Si1 O1 K1 9.6(3) . . . . ?
O3 Si1 O2 C13 -95.6(7) . . . . ?
O4 Si2 O5 C30 -32.7(8) . . . . ?
O4 Si2 O6 K2 -8.4(3) . . . . ?
O4 Si2 O6 C34 -175.3(8) . . . . ?
O4 Si2 C29 K1 43.4(4) . . . . ?
O4 Si2 C29 C24 -32.1(8) . . . . ?
O4 Si2 C29 C28 139.6(7) . . . . ?
O5 Si2 O4 Ce1 149.3(4) . . . . ?
O5 Si2 O4 K2 -103.5(3) . . . . ?
O5 Si2 O6 K2 111.4(3) . . . . ?
O5 Si2 O6 C34 -55.5(8) . . . . ?
O5 Si2 C29 K1 -83.2(4) . . . . ?
O5 Si2 C29 C24 -158.7(7) . . . . ?
O5 Si2 C29 C28 13.0(8) . . . . ?
O6 Si2 O4 Ce1 -99.0(5) . . . . ?
O6 Si2 O4 K2 8.1(3) . . . . ?
O6 Si2 O5 C30 -145.8(7) . . . . ?
O6 Si2 C29 K1 163.3(3) . . . . ?
O6 Si2 C29 C24 87.8(8) . . . . ?
O6 Si2 C29 C28 -100.5(7) . . . . ?
O7 Si3 O8 C47 42.5(10) . . . . ?
O7 Si3 O9 C51 170.6(7) . . . . ?
O7 Si3 C46 K2 36.3(3) . . . . ?
O7 Si3 C46 C41 -38.0(9) . . . . ?
O7 Si3 C46 C45 129.9(8) . . . . ?
O8 Si3 O7 Ce1 174.0(4) . . . . ?
O8 Si3 O7 K2 68.0(3) . . . . ?
O8 Si3 O9 C51 -64.6(9) . . . . ?
O8 Si3 C46 K2 -82.6(3) . . . . ?
O8 Si3 C46 C41 -156.9(8) . . . . ?
O8 Si3 C46 C45 11.0(9) . . . . ?
O9 Si3 O7 Ce1 -63.3(5) . . . . ?
O9 Si3 O7 K2 -169.3(3) . . . . ?
O9 Si3 O8 C47 -81.5(9) . . . . ?
O9 Si3 C46 K2 161.0(2) . . . . ?
O9 Si3 C46 C41 86.7(8) . . . . ?
O9 Si3 C46 C45 -105.4(8) . . . . ?
C1 C2 C3 Ce1 -51.0(7) . . . . ?
C1 C2 C3 C4 18.0(11) . . . . ?
C1 C2 C3 C24 -167.3(8) . . . . ?
C1 C7 C8 C9 177.5(8) . . . . ?
C1 C7 C12 Si1 -3.1(11) . . . . ?
C1 C7 C12 C11 -176.1(7) . . . . ?
C2 C1 C6 Ce1 66.0(7) . . . . ?
C2 C1 C6 C5 -9.6(11) . . . . ?
C2 C1 C7 C8 140.1(8) . . . . ?
C2 C1 C7 C12 -44.8(11) . . . . ?
C2 C3 C4 Ce1 -70.8(6) . . . . ?
C2 C3 C4 C5 -10.5(11) . . . . ?
C2 C3 C24 K1 52.5(8) . . . . ?
C2 C3 C24 C25 -28.1(12) . . . . ?
C2 C3 C24 C29 148.7(8) . . . . ?
C3 C4 C5 Ce1 -59.5(7) . . . . ?
C3 C4 C5 C6 -6.9(12) . . . . ?
C3 C4 C5 C41 176.1(7) . . . . ?
C3 C24 C25 K1 101.8(7) . . . . ?
C3 C24 C25 C26 -177.4(8) . . . . ?
C3 C24 C29 K1 -108.1(8) . . . . ?
C3 C24 C29 Si2 -12.1(12) . . . . ?
C3 C24 C29 C28 176.3(8) . . . . ?
C4 C3 C24 K1 -133.1(7) . . . . ?
C4 C3 C24 C25 146.3(8) . . . . ?
C4 C3 C24 C29 -36.9(13) . . . . ?
C4 C5 C6 Ce1 -57.0(7) . . . . ?
C4 C5 C6 C1 16.7(11) . . . . ?
C4 C5 C41 K2 61.5(7) . . . . ?
C4 C5 C41 C42 -47.2(12) . . . . ?
C4 C5 C41 C46 130.1(9) . . . . ?
C5 C41 C42 C43 176.7(10) . . . . ?
C5 C41 C46 K2 -79.5(9) . . . . ?
C5 C41 C46 Si3 -8.4(13) . . . . ?
C5 C41 C46 C45 -176.5(9) . . . . ?
C6 C1 C2 Ce1 -59.9(7) . . . . ?
C6 C1 C2 C3 -8.0(12) . . . . ?
C6 C1 C7 C8 -44.8(11) . . . . ?
C6 C1 C7 C12 130.4(8) . . . . ?
C6 C5 C41 K2 -115.5(7) . . . . ?
C6 C5 C41 C42 135.9(9) . . . . ?
C6 C5 C41 C46 -46.9(13) . . . . ?
C7 C1 C2 Ce1 115.2(7) . . . . ?
C7 C1 C2 C3 167.0(7) . . . . ?
C7 C1 C6 Ce1 -109.1(7) . . . . ?
C7 C1 C6 C5 175.3(7) . . . . ?
C7 C8 C9 C10 -0.9(14) . . . . ?
C8 C7 C12 Si1 171.9(6) . . . . ?
C8 C7 C12 C11 -1.1(11) . . . . ?
C8 C9 C10 C11 -1.4(15) . . . . ?
C9 C10 C11 C12 2.6(15) . . . . ?
C10 C11 C12 Si1 -175.1(8) . . . . ?
C10 C11 C12 C7 -1.4(13) . . . . ?
C12 Si1 O1 Ce1 9.0(5) . . . . ?
C12 Si1 O1 K1 133.9(3) . . . . ?
C12 Si1 O2 C13 145.7(7) . . . . ?
C12 Si1 O3 K1 -136.1(3) . . . . ?
C12 Si1 O3 C17 63.6(8) . . . . ?
C12 C7 C8 C9 2.3(13) . . . . ?
C24 C3 C4 Ce1 114.5(8) . . . . ?
C24 C3 C4 C5 174.8(8) . . . . ?
C24 C25 C26 K1 -75.8(8) . . . . ?
C24 C25 C26 C27 -1.4(15) . . . . ?
C25 C24 C29 K1 68.8(7) . . . . ?
C25 C24 C29 Si2 164.8(6) . . . . ?
C25 C24 C29 C28 -6.8(12) . . . . ?
C25 C26 C27 C28 -1.4(15) . . . . ?
C26 C27 C28 K1 -55.5(8) . . . . ?
C26 C27 C28 C29 -0.2(15) . . . . ?
C27 C28 C29 K1 -60.4(9) . . . . ?
C27 C28 C29 Si2 -167.7(8) . . . . ?
C27 C28 C29 C24 4.5(14) . . . . ?
C29 Si2 O4 Ce1 26.5(6) . . . . ?
C29 Si2 O4 K2 133.6(3) . . . . ?
C29 Si2 O5 C30 92.7(7) . . . . ?
C29 Si2 O6 K2 -132.3(4) . . . . ?
C29 Si2 O6 C34 60.8(9) . . . . ?
C29 C24 C25 K1 -75.3(7) . . . . ?
C29 C24 C25 C26 5.5(13) . . . . ?
C41 C5 C6 Ce1 119.9(8) . . . . ?
C41 C5 C6 C1 -166.4(8) . . . . ?
C41 C42 C43 C44 -0.2(17) . . . . ?
C42 C41 C46 K2 97.7(8) . . . . ?
C42 C41 C46 Si3 168.8(7) . . . . ?
C42 C41 C46 C45 0.7(14) . . . . ?
C42 C43 C44 C45 1.1(18) . . . . ?
C43 C44 C45 C46 -1.2(18) . . . . ?
C44 C45 C46 K2 -87.7(11) . . . . ?
C44 C45 C46 Si3 -168.5(9) . . . . ?
C44 C45 C46 C41 0.2(15) . . . . ?
C46 Si3 O7 Ce1 62.7(5) . . . . ?
C46 Si3 O7 K2 -43.3(4) . . . . ?
C46 Si3 O8 C47 158.8(9) . . . . ?
C46 Si3 O9 C51 47.1(9) . . . . ?
C46 C41 C42 C43 -0.7(16) . . . . ?
C55 O10 C57 C58 -174.7(8) . . . . ?
C57 O10 C55 C56 178.3(7) . . . . ?
C59 O11 C61 C62 175.5(9) . . . . ?
C61 O11 C59 C60 71.5(13) . . . . ?
C63 O12 C65 C66 -169(2) . . . . ?
C63 O12 C67 C68 74(3) . . . . ?
C65 O12 C63 C64 -175.7(16) . . . . ?
C67 O12 C63 C64 157(2) . . . . ?
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
1.0000 -0.0000 -1.0000 -0.0299 0.0245 -0.0654
-1.0000 0.0000 1.0000 0.0299 -0.0245 0.0654
0.0000 -2.0000 -1.0001 -0.2047 0.1629 0.1119
-1.0000 -2.0000 -0.0001 -0.1747 0.1384 0.1774
-0.0000 2.0000 1.0001 0.2047 -0.1629 -0.1119
1.0000 2.0000 0.0001 0.1747 -0.1384 -0.1774
2.0000 -0.0000 -1.0001 -0.0700 -0.0058 -0.1039
1.0000 -0.0000 -0.0000 -0.0400 -0.0303 -0.0385
1.0000 -0.0000 0.9999 -0.0502 -0.0851 -0.0116
-0.0051 -2.5206 15.1345 -0.4237 -0.6935 0.5827
-1.0001 0.0000 -1.9999 0.0603 0.1400 -0.0153
-2.0001 1.0000 -0.9998 0.1976 0.0614 -0.0193
-13.0568 1.4472 -5.6926 0.7359 0.6296 0.2490
-15.7279 -1.9824 4.8948 0.3674 0.3154 0.8750
0.0001 5.0000 12.0002 0.4154 -0.9282 -0.0241
9.0004 -3.0001 8.9993 -0.7737 -0.6041 0.1041
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 0.500 0.500 205.1 39.8 '0.8 toluene'
2 0.500 0.000 0.000 205.1 39.8 '0.8 toluene'
