#------------------------------------------------------------------------------
#$Date: 2024-10-06 09:25:44 +0300 (Sun, 06 Oct 2024) $
#$Revision: 295157 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/33/7133324.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_7133324
loop_
_publ_author_name
'Katzer, Nicholas J.'
'Kaur, Mandeep'
'Sen, Asmita'
'Nimaiyar, Rupal'
'Autschbach, Jochen'
'Arnold, Polly L.'
'Hintermair, Ulrich'
_publ_section_title
;
 Tetraphenylpentalenide organolanthanide complexes.
;
_journal_issue                   72
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9749
_journal_page_last               9752
_journal_paper_doi               10.1039/d4cc02570a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C64 H44 Ce, C16 H40 K O8'
_chemical_formula_sum            'C80 H84 Ce K O8'
_chemical_formula_weight         1352.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-14
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-05-23 deposited with the CCDC.	2024-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.0560(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.84690(10)
_cell_length_b                   10.17870(10)
_cell_length_c                   21.4308(2)
_cell_measurement_reflns_used    44064
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      79.5520
_cell_measurement_theta_min      3.3650
_cell_volume                     3448.15(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.99a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.99a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.99a (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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -56.00  25.00   0.50    1.47    --  -47.94  57.00 -90.00  162
  2  ω     -2.00  26.00   0.50    1.47    --  -47.94  19.00 -90.00   56
  3  ω    -63.00  25.00   0.50    1.47    --  -47.94  57.00  30.00  176
  4  ω   -118.00 -86.00   0.50    1.47    --  -47.94 -46.00-156.31   64
  5  ω    -62.00 -36.00   0.50    1.47    --  -47.94 -46.00-156.31   52
  6  ω    -16.00  19.00   0.50    1.47    --  -47.94  19.00 -30.00   70
  7  ω    -16.00  24.00   0.50    1.47    --  -47.94  19.00-180.00   80
  8  ω    -81.00 -33.00   0.50    1.47    --  -47.94 125.00  90.00   96
  9  ω    -85.00 -37.00   0.50    1.47    --  -47.94 -41.00 -95.88   96
 10  ω   -120.00 -94.00   0.50    1.47    --  -47.94 -41.00 -95.88   52
 11  ω    -26.00  -1.00   0.50    1.47    --   47.94 -19.00 -30.00   50
 12  ω     46.00  86.00   0.50    1.47    --   47.94-125.00 150.00   80
 13  ω   -139.00-106.00   0.50    5.89    --  -91.75 -61.00-150.00   66
 14  ω   -108.00 -80.00   0.50    5.89    --  -91.75 -45.00 -60.00   56
 15  ω    111.00 172.00   0.50    5.89    --  113.25  77.00  60.00  122
 16  ω     56.00  94.00   0.50    5.89    --  113.25 -94.00  60.00   76
 17  ω     83.00 111.00   0.50    5.89    --  113.25 -82.00  51.08   56
 18  ω    150.00 175.00   0.50    5.89    --  113.25  77.00 150.00   50
 19  ω    104.00 129.00   0.50    5.89    --  113.25  15.00  30.00   50
 20  ω    146.00 178.00   0.50    5.89    --  113.25 103.00-165.77   64
 21  ω     48.00 107.00   0.50    5.89    --  113.25-105.00 -84.56  118
 22  ω    102.00 136.00   0.50    5.89    --  113.25  30.00  30.00   68
 23  ω    132.00 158.00   0.50    5.89    --  113.25  15.00  30.00   52
 24  ω     42.00  74.00   0.50    5.89    --  113.25 -94.00 -60.00   64
 25  ω     79.00 106.00   0.50    5.89    --  113.25 -94.00 -60.00   54
 26  ω    127.00 165.00   0.50    5.89    --  113.25 125.00 -90.00   76
 27  ω     43.00  71.00   0.50    5.89    --  113.25 -77.00-180.00   56
 28  ω    103.00 129.00   0.50    5.89    --  113.25 -77.00-180.00   52
 29  ω     42.00  67.00   0.50    5.89    --  113.25 -61.00 -60.00   50
 30  ω     85.00 111.00   0.50    5.89    --  113.25-125.00 -30.00   52
 31  ω     42.00 104.00   0.50    5.89    --  113.25 -94.00-120.00  124
 32  ω     43.00  68.00   0.50    5.89    --  113.25 -61.00   0.00   50
 33  ω    134.00 163.00   0.50    5.89    --  113.25  15.00-120.00   58
 34  ω     48.00  84.00   0.50    5.89    --  113.25-125.00 -60.00   72
 35  ω     71.00 106.00   0.50    5.89    --  113.25 -94.00-180.00   70
 36  ω    109.00 139.00   0.50    5.89    --  113.25 -86.00  94.10   60
 37  ω     42.00  67.00   0.50    5.89    --  113.25 -94.00-180.00   50
 38  ω    111.00 141.00   0.50    5.89    --  113.25  77.00-180.00   60
 39  ω    110.00 139.00   0.50    5.89    --  113.25  77.00-120.00   58
 40  ω    114.00 139.00   0.50    5.89    --  113.25  61.00-180.00   50
 41  ω    101.00 166.00   0.50    5.89    --  113.25  45.00  60.00  130
 42  ω    123.00 149.00   0.50    5.89    --  113.25  30.00 150.00   52
 43  ω     49.00 106.00   0.50    5.89    --  113.25 -94.00  90.00  114
 44  ω     56.00  82.00   0.50    5.89    --  113.25 -77.00 -60.00   52
 45  ω    120.00 168.00   0.50    5.89    --  113.25  77.00 -90.00   96
 46  ω     91.00 131.00   0.50    5.89    --  113.25 -77.00  60.00   80
 47  ω    148.00 174.00   0.50    5.89    --  113.25  30.00  30.00   52
 48  ω     42.00  70.00   0.50    5.89    --  113.25 -61.00-150.00   56
 49  ω     81.00 106.00   0.50    5.89    --  113.25 -94.00  30.00   50
 50  ω     43.00  68.00   0.50    5.89    --  113.25 -77.00 -90.00   50
 51  ω    100.00 126.00   0.50    5.89    --  113.25 -77.00 -90.00   52
 52  ω     43.00  73.00   0.50    5.89    --  113.25 -77.00 -30.00   60
 53  ω     92.00 121.00   0.50    5.89    --  113.25 -77.00 -30.00   58
 54  ω     76.00 106.00   0.50    5.89    --  113.25 -94.00 150.00   60
 55  ω    105.00 145.00   0.50    5.89    --  113.25  45.00-120.00   80
 56  ω     42.00  71.00   0.50    5.89    --  113.25 -61.00  90.00   58
 57  ω    141.00 167.00   0.50    5.89    --  113.25 125.00-120.00   52
 58  ω    145.00 177.00   0.50    5.89    --  113.25  77.00-150.00   64
 59  ω    123.00 157.00   0.50    5.89    --  113.25  45.00 -30.00   68
 60  ω     53.00 110.00   0.50    5.89    --  113.25-125.00 120.00  114
 61  ω     46.00  73.00   0.50    5.89    --  113.25 -77.00   0.00   54
 62  ω     42.00  67.00   0.50    5.89    --  113.25 -61.00 150.00   50
 63  ω     44.00  85.00   0.50    5.89    --  113.25-125.00 150.00   82
 64  ω     98.00 123.00   0.50    5.89    --  113.25 125.00-150.00   50
 65  ω    103.00 159.00   0.50    5.89    --  113.25  45.00 150.00  112
 66  ω    108.00 134.00   0.50    5.89    --  113.25  61.00  30.00   52
 67  ω     64.00 105.00   0.50    5.89    --  113.25 -94.00   0.00   82
 68  ω    135.00 161.00   0.50    5.89    --  113.25 125.00-150.00   52
 69  ω    102.00 170.00   0.50    5.89    --  113.25 125.00   0.00  136
 70  ω    102.00 151.00   0.50    5.89    --  113.25  15.00 -30.00   98
 71  ω    110.00 160.00   0.50    5.89    --  113.25  77.00 -30.00  100
 72  ω    142.00 168.00   0.50    5.89    --  113.25  30.00  90.00   52
 73  ω     95.00 121.00   0.50    5.89    --  113.25 125.00 -30.00   52
 74  ω    153.00 178.00   0.50    5.89    --  113.25  61.00   0.00   50
 75  ω     55.00  94.00   0.50    5.89    --  113.25 -94.00-150.00   78
 76  ω     46.00  77.00   0.50    5.89    --  113.25 -94.00 -30.00   62
 77  ω     50.00  82.00   0.50    5.89    --  113.25-125.00-150.00   64
 78  ω    107.00 144.00   0.50    5.89    --  113.25  61.00   0.00   74
 79  ω     55.00  80.00   0.50    5.89    --  113.25 -77.00  30.00   50
 80  ω     42.00  67.00   0.50    5.89    --  113.25 -61.00 -30.00   50
 81  ω    113.00 139.00   0.50    5.89    --  113.25  99.00 -32.56   52
 82  ω     45.00  71.00   0.50    5.89    --  113.25 -61.00 120.00   52
 83  ω    127.00 153.00   0.50    5.89    --  113.25  61.00-120.00   52
 84  ω    103.00 148.00   0.50    5.89    --  113.25  45.00 120.00   90
 85  ω    108.00 152.00   0.50    5.89    --  113.25  30.00 -30.00   88
 86  ω     50.00  76.00   0.50    5.89    --  113.25 -86.00  94.10   52
 87  ω    100.00 125.00   0.50    5.89    --  113.25 125.00  60.00   50
 88  ω    141.00 167.00   0.50    5.89    --  113.25 125.00  60.00   52
 89  ω     65.00  91.00   0.50    5.89    --  113.25 -77.00-150.00   52
 90  ω     73.00 106.00   0.50    5.89    --  113.25 -99.00 -20.49   66
 91  ω    108.00 133.00   0.50    5.89    --  113.25 -77.00  90.00   50
 92  ω     51.00  76.00   0.50    5.89    --  113.25 -77.00 120.00   50
 93  ω     68.00 106.00   0.50    5.89    --  113.25 -97.00 131.03   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0877284000
_diffrn_orient_matrix_UB_12      -0.0471973000
_diffrn_orient_matrix_UB_13      0.0263925000
_diffrn_orient_matrix_UB_21      0.0241870000
_diffrn_orient_matrix_UB_22      -0.0308767000
_diffrn_orient_matrix_UB_23      -0.0668321000
_diffrn_orient_matrix_UB_31      0.0347754000
_diffrn_orient_matrix_UB_32      0.1404739000
_diffrn_orient_matrix_UB_33      -0.0057747000
_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  0.0666
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            75093
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.960
_diffrn_reflns_theta_min         3.358
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.077
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.342
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.99a (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            gold
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       needle
_exptl_crystal_F_000             1410
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.974
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         7501
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0334
_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)+(0.0271P)²+4.3944P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0803
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7284
_reflns_number_total             7501
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4cc02570a2.cif
_cod_data_source_block           pla23085_refinalized
_cod_depositor_comments
'Adding full bibliography for 7133320--7133330.cif.'
_cod_database_code               7133324
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ce K O8 C96 H144'
_chemical_oxdiff_usercomment     'NJK-07-051 from DME'
_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   0.839
_shelx_estimated_absorpt_t_min   0.121
_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.a Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C35(H35A,H35B), C39(H39A,H39B), C38(H38A,H38B)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C5(H5), C2(H2), C22(H22), C20(H20), C11(H11), C26(H26), C14(H14),
 C28(H28), C23(H23), C19(H19), C32(H32), C13(H13), C16(H16), C25(H25), C31(H31),
  C24(H24), C17(H17), C29(H29), C30(H30), C18(H18), C12(H12)
2.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C33(H33A,H33B,H33C), C36(H36A,H36B,H36C), C37(H37A,H37B,
 H37C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.485
_oxdiff_exptl_absorpt_empirical_full_min 0.741
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce1 Ce 0.250000 0.41717(2) 0.250000 0.02185(6) Uani 1 2 d S T P . .
K1 K 0.750000 -0.07800(8) 0.250000 0.03247(15) Uani 1 2 d S T P . .
O1 O 0.63804(15) -0.2750(2) 0.21231(11) 0.0530(6) Uani 1 1 d . . . . .
O2 O 0.66308(15) -0.2213(3) 0.34033(11) 0.0593(6) Uani 1 1 d . . . . .
O4 O 0.81677(16) 0.0539(2) 0.36326(12) 0.0589(6) Uani 1 1 d . . . . .
O3 O 0.66533(15) 0.1296(3) 0.29920(13) 0.0649(7) Uani 1 1 d . . . . .
C9 C 0.41093(15) 0.2996(2) 0.12940(11) 0.0263(5) Uani 1 1 d . . . . .
C4 C 0.38166(14) 0.4929(2) 0.33873(11) 0.0252(4) Uani 1 1 d . . . . .
C10 C 0.36737(16) 0.2084(2) 0.08991(12) 0.0286(5) Uani 1 1 d . . . . .
H10 H 0.322346 0.158823 0.105096 0.034 Uiso 1 1 calc R U . . .
C21 C 0.36584(15) 0.5000(2) 0.40546(12) 0.0274(5) Uani 1 1 d . . . . .
C8 C 0.39953(14) 0.3801(2) 0.30030(11) 0.0243(4) Uani 1 1 d . . . . .
C27 C 0.38708(14) 0.6570(2) 0.18216(12) 0.0275(5) Uani 1 1 d . . . . .
C5 C 0.38097(14) 0.6029(2) 0.29817(12) 0.0274(5) Uani 1 1 d . . . . .
H5 H 0.372567 0.690861 0.311258 0.033 Uiso 1 1 calc R U . . .
C3 C 0.37802(14) 0.2413(2) 0.29734(11) 0.0242(4) Uani 1 1 d . . . . .
C15 C 0.37456(14) 0.1469(2) 0.34833(11) 0.0258(5) Uani 1 1 d . . . . .
C2 C 0.37326(14) 0.2075(2) 0.23351(11) 0.0236(4) Uani 1 1 d . . . . .
H2 H 0.358790 0.122386 0.218031 0.028 Uiso 1 1 calc R U . . .
C22 C 0.40430(18) 0.5977(3) 0.44355(13) 0.0357(6) Uani 1 1 d . . . . .
H22 H 0.441708 0.658542 0.426295 0.043 Uiso 1 1 calc R U . . .
C20 C 0.33083(16) 0.0269(2) 0.34062(13) 0.0312(5) Uani 1 1 d . . . . .
H20 H 0.300390 0.008030 0.301878 0.037 Uiso 1 1 calc R U . . .
C6 C 0.39424(15) 0.5665(2) 0.23597(12) 0.0261(5) Uani 1 1 d . . . . .
C11 C 0.38936(18) 0.1897(3) 0.02879(12) 0.0345(5) Uani 1 1 d . . . . .
H11 H 0.359157 0.127713 0.002690 0.041 Uiso 1 1 calc R U . . .
C26 C 0.31004(16) 0.4137(2) 0.43268(12) 0.0310(5) Uani 1 1 d . . . . .
H26 H 0.283159 0.346462 0.407770 0.037 Uiso 1 1 calc R U . . .
C7 C 0.40857(14) 0.4261(2) 0.23719(11) 0.0252(4) Uani 1 1 d . . . . .
C1 C 0.39257(14) 0.3153(2) 0.19488(11) 0.0240(4) Uani 1 1 d . . . . .
C14 C 0.47665(16) 0.3713(2) 0.10486(13) 0.0324(5) Uani 1 1 d . . . . .
H14 H 0.506761 0.434279 0.130440 0.039 Uiso 1 1 calc R U . . .
C28 C 0.35406(16) 0.6155(2) 0.12317(12) 0.0302(5) Uani 1 1 d . . . . .
H28 H 0.338090 0.526202 0.117242 0.036 Uiso 1 1 calc R U . . .
C23 C 0.3884(2) 0.6068(3) 0.50652(14) 0.0426(6) Uani 1 1 d . . . . .
H23 H 0.415780 0.672733 0.531957 0.051 Uiso 1 1 calc R U . . .
C19 C 0.3316(2) -0.0639(3) 0.38879(15) 0.0417(7) Uani 1 1 d . . . . .
H19 H 0.302083 -0.144640 0.382726 0.050 Uiso 1 1 calc R U . . .
C32 C 0.40931(16) 0.7896(2) 0.18917(14) 0.0338(5) Uani 1 1 d . . . . .
H32 H 0.430556 0.821212 0.228934 0.041 Uiso 1 1 calc R U . . .
C13 C 0.49853(18) 0.3518(3) 0.04392(13) 0.0375(6) Uani 1 1 d . . . . .
H13 H 0.543484 0.401048 0.028396 0.045 Uiso 1 1 calc R U . . .
C16 C 0.41879(18) 0.1705(3) 0.40602(13) 0.0353(5) Uani 1 1 d . . . . .
H16 H 0.449239 0.250375 0.412269 0.042 Uiso 1 1 calc R U . . .
C25 C 0.2932(2) 0.4242(3) 0.49517(13) 0.0396(6) Uani 1 1 d . . . . .
H25 H 0.254490 0.365412 0.512419 0.047 Uiso 1 1 calc R U . . .
C31 C 0.40070(19) 0.8756(3) 0.13876(15) 0.0410(7) Uani 1 1 d . . . . .
H31 H 0.417166 0.964820 0.144261 0.049 Uiso 1 1 calc R U . . .
C24 C 0.3328(2) 0.5205(3) 0.53237(14) 0.0451(7) Uani 1 1 d . . . . .
H24 H 0.322022 0.527258 0.575298 0.054 Uiso 1 1 calc R U . . .
C17 C 0.4191(3) 0.0797(3) 0.45435(14) 0.0506(8) Uani 1 1 d . . . . .
H17 H 0.449393 0.097957 0.493245 0.061 Uiso 1 1 calc R U . . .
C29 C 0.34408(19) 0.7021(3) 0.07297(14) 0.0386(6) Uani 1 1 d . . . . .
H29 H 0.320665 0.672093 0.033494 0.046 Uiso 1 1 calc R U . . .
C30 C 0.3684(2) 0.8327(3) 0.08066(15) 0.0441(7) Uani 1 1 d . . . . .
H30 H 0.362929 0.891863 0.046327 0.053 Uiso 1 1 calc R U . . .
C18 C 0.3753(3) -0.0376(3) 0.44590(15) 0.0534(9) Uani 1 1 d . . . . .
H18 H 0.375211 -0.099721 0.478994 0.064 Uiso 1 1 calc R U . . .
C12 C 0.45512(19) 0.2610(3) 0.00561(13) 0.0386(6) Uani 1 1 d . . . . .
H12 H 0.470161 0.247564 -0.036044 0.046 Uiso 1 1 calc R U . . .
C34 C 0.6160(2) -0.3676(4) 0.25808(18) 0.0571(9) Uani 1 1 d . . . . .
H34A H 0.664439 -0.426889 0.268757 0.068 Uiso 1 1 calc R U . . .
H34B H 0.567573 -0.421483 0.241401 0.068 Uiso 1 1 calc R U . . .
C40 C 0.9032(2) 0.0409(4) 0.3825(2) 0.0669(11) Uani 1 1 d . . . . .
H40A H 0.919911 -0.051510 0.379812 0.100 Uiso 1 1 calc R U . . .
H40B H 0.913005 0.071191 0.425862 0.100 Uiso 1 1 calc R U . . .
H40C H 0.936945 0.094006 0.355372 0.100 Uiso 1 1 calc R U . . .
C35 C 0.5931(2) -0.2956(4) 0.31508(18) 0.0630(10) Uani 1 1 d . . . . .
H35A H 0.544797 -0.236218 0.304174 0.076 Uiso 1 1 calc R U . . .
H35B H 0.575650 -0.359079 0.346699 0.076 Uiso 1 1 calc R U . . .
C33 C 0.6427(3) -0.3352(4) 0.15333(18) 0.0673(11) Uani 1 1 d . . . . .
H33A H 0.663845 -0.271684 0.123818 0.101 Uiso 1 1 calc R U . . .
H33B H 0.586263 -0.365200 0.137897 0.101 Uiso 1 1 calc R U . . .
H33C H 0.681198 -0.410544 0.157325 0.101 Uiso 1 1 calc R U . . .
C36 C 0.6439(3) -0.1546(5) 0.39613(18) 0.0740(12) Uani 1 1 d . . . . .
H36A H 0.692644 -0.101493 0.411403 0.111 Uiso 1 1 calc R U . . .
H36B H 0.631155 -0.219179 0.428062 0.111 Uiso 1 1 calc R U . . .
H36C H 0.594781 -0.097451 0.387251 0.111 Uiso 1 1 calc R U . . .
C37 C 0.5762(3) 0.1407(6) 0.2874(3) 0.0983(19) Uani 1 1 d . . . . .
H37A H 0.557793 0.086749 0.251106 0.147 Uiso 1 1 calc R U . . .
H37B H 0.561313 0.232735 0.278893 0.147 Uiso 1 1 calc R U . . .
H37C H 0.548204 0.110375 0.324091 0.147 Uiso 1 1 calc R U . . .
C39 C 0.7901(3) 0.1865(4) 0.3611(2) 0.0760(12) Uani 1 1 d . . . . .
H39A H 0.814751 0.231712 0.325713 0.091 Uiso 1 1 calc R U . . .
H39B H 0.810516 0.231597 0.400235 0.091 Uiso 1 1 calc R U . . .
C38 C 0.6959(3) 0.1940(5) 0.3533(3) 0.0885(15) Uani 1 1 d . . . . .
H38A H 0.671482 0.153499 0.389931 0.106 Uiso 1 1 calc R U . . .
H38B H 0.678083 0.287225 0.351128 0.106 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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 -2 0.0198
-1 0 2 0.0367
1 0 0 0.0213
-1 0 0 0.0051
2 1 0 0.1108
2 2 1 0.1456
-1 -2 1 0.3846
2 0 1 0.0318
0 2 1 0.1661
-1 0 -1 0.0097
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
C4 Ce1 C4 148.39(9) . 2 ?
C4 Ce1 C3 152.44(7) 2 . ?
C4 Ce1 C3 57.11(7) . . ?
C4 Ce1 C3 57.11(7) 2 2 ?
C4 Ce1 C3 152.44(7) . 2 ?
C8 Ce1 C4 160.00(7) . 2 ?
C8 Ce1 C4 160.00(7) 2 . ?
C8 Ce1 C4 30.76(7) . . ?
C8 Ce1 C4 30.76(7) 2 2 ?
C8 Ce1 C8 163.04(10) 2 . ?
C8 Ce1 C3 132.38(7) . 2 ?
C8 Ce1 C3 30.68(6) 2 2 ?
C8 Ce1 C3 132.38(7) 2 . ?
C8 Ce1 C3 30.68(6) . . ?
C8 Ce1 C6 141.14(7) . 2 ?
C8 Ce1 C6 51.88(7) . . ?
C8 Ce1 C6 51.88(7) 2 2 ?
C8 Ce1 C6 141.14(7) 2 . ?
C8 Ce1 C1 120.95(7) 2 . ?
C8 Ce1 C1 51.48(7) . . ?
C8 Ce1 C1 51.48(7) 2 2 ?
C8 Ce1 C1 120.95(7) . 2 ?
C3 Ce1 C3 101.82(9) . 2 ?
C6 Ce1 C4 110.57(7) . 2 ?
C6 Ce1 C4 49.50(7) . . ?
C6 Ce1 C4 110.57(7) 2 . ?
C6 Ce1 C4 49.50(7) 2 2 ?
C6 Ce1 C3 151.50(7) . 2 ?
C6 Ce1 C3 79.12(7) 2 2 ?
C6 Ce1 C3 151.50(7) 2 . ?
C6 Ce1 C3 79.11(7) . . ?
C6 Ce1 C6 113.67(9) . 2 ?
C6 Ce1 C1 159.37(7) 2 . ?
C6 Ce1 C1 57.75(6) 2 2 ?
C6 Ce1 C1 159.37(7) . 2 ?
C6 Ce1 C1 57.75(6) . . ?
C7 Ce1 C4 51.45(7) 2 2 ?
C7 Ce1 C4 127.15(7) 2 . ?
C7 Ce1 C4 51.45(7) . . ?
C7 Ce1 C4 127.15(7) . 2 ?
C7 Ce1 C8 148.20(7) . 2 ?
C7 Ce1 C8 148.20(7) 2 . ?
C7 Ce1 C8 32.92(7) . . ?
C7 Ce1 C8 32.92(7) 2 2 ?
C7 Ce1 C3 132.00(7) . 2 ?
C7 Ce1 C3 51.37(7) 2 2 ?
C7 Ce1 C3 132.00(7) 2 . ?
C7 Ce1 C3 51.37(7) . . ?
C7 Ce1 C6 144.78(7) 2 . ?
C7 Ce1 C6 31.15(6) 2 2 ?
C7 Ce1 C6 31.15(6) . . ?
C7 Ce1 C6 144.77(7) . 2 ?
C7 Ce1 C7 175.92(10) 2 . ?
C7 Ce1 C1 30.99(7) 2 2 ?
C7 Ce1 C1 152.06(7) 2 . ?
C7 Ce1 C1 152.06(7) . 2 ?
C7 Ce1 C1 30.99(7) . . ?
C1 Ce1 C4 78.88(7) . . ?
C1 Ce1 C4 113.16(7) . 2 ?
C1 Ce1 C4 113.15(7) 2 . ?
C1 Ce1 C4 78.88(7) 2 2 ?
C1 Ce1 C3 101.07(6) . 2 ?
C1 Ce1 C3 49.03(7) . . ?
C1 Ce1 C3 49.03(7) 2 2 ?
C1 Ce1 C3 101.07(6) 2 . ?
C1 Ce1 C1 136.85(9) . 2 ?
O1 K1 O1 86.82(11) . 2_655 ?
O1 K1 O2 59.75(7) . . ?
O1 K1 O2 76.20(8) . 2_655 ?
O1 K1 O2 76.20(8) 2_655 . ?
O1 K1 O2 59.75(7) 2_655 2_655 ?
O1 K1 O4 140.21(7) . . ?
O1 K1 O4 140.21(7) 2_655 2_655 ?
O1 K1 O4 84.42(7) . 2_655 ?
O1 K1 O4 84.42(7) 2_655 . ?
O2 K1 O2 118.54(12) . 2_655 ?
O2 K1 O4 129.62(7) . 2_655 ?
O2 K1 O4 129.62(7) 2_655 . ?
O2 K1 O4 80.47(8) . . ?
O2 K1 O4 80.47(8) 2_655 2_655 ?
O4 K1 O4 124.97(11) . 2_655 ?
O3 K1 O1 110.43(8) . . ?
O3 K1 O1 110.43(8) 2_655 2_655 ?
O3 K1 O1 140.01(7) 2_655 . ?
O3 K1 O1 140.01(7) . 2_655 ?
O3 K1 O2 82.00(8) 2_655 2_655 ?
O3 K1 O2 157.47(9) 2_655 . ?
O3 K1 O2 82.00(8) . . ?
O3 K1 O2 157.47(9) . 2_655 ?
O3 K1 O4 78.86(8) 2_655 . ?
O3 K1 O4 78.86(8) . 2_655 ?
O3 K1 O4 58.94(8) 2_655 2_655 ?
O3 K1 O4 58.94(8) . . ?
O3 K1 O3 79.73(12) . 2_655 ?
C34 O1 K1 117.62(19) . . ?
C33 O1 K1 120.3(2) . . ?
C33 O1 C34 111.2(3) . . ?
C35 O2 K1 114.56(19) . . ?
C35 O2 C36 111.5(3) . . ?
C36 O2 K1 117.8(2) . . ?
C40 O4 K1 119.4(2) . . ?
C40 O4 C39 112.4(3) . . ?
C39 O4 K1 108.9(2) . . ?
C37 O3 K1 119.9(3) . . ?
C38 O3 K1 122.1(2) . . ?
C38 O3 C37 113.2(4) . . ?
C10 C9 C1 121.9(2) . . ?
C14 C9 C10 117.6(2) . . ?
C14 C9 C1 120.4(2) . . ?
C21 C4 Ce1 119.92(15) . . ?
C8 C4 Ce1 64.39(12) . . ?
C8 C4 C21 130.1(2) . . ?
C5 C4 Ce1 80.20(13) . . ?
C5 C4 C21 124.2(2) . . ?
C5 C4 C8 105.7(2) . . ?
C9 C10 H10 119.6 . . ?
C11 C10 C9 120.8(2) . . ?
C11 C10 H10 119.6 . . ?
C22 C21 C4 120.4(2) . . ?
C22 C21 C26 117.7(2) . . ?
C26 C21 C4 121.9(2) . . ?
C4 C8 Ce1 84.86(13) . . ?
C4 C8 C3 137.6(2) . . ?
C3 C8 Ce1 85.28(13) . . ?
C7 C8 Ce1 73.07(13) . . ?
C7 C8 C4 108.07(19) . . ?
C7 C8 C3 108.2(2) . . ?
C28 C27 C6 121.5(2) . . ?
C28 C27 C32 117.6(2) . . ?
C32 C27 C6 120.9(2) . . ?
Ce1 C5 H5 126.8 . . ?
C4 C5 Ce1 71.44(12) . . ?
C4 C5 H5 124.0 . . ?
C6 C5 Ce1 69.44(13) . . ?
C6 C5 C4 112.1(2) . . ?
C6 C5 H5 124.0 . . ?
C8 C3 Ce1 64.05(12) . . ?
C8 C3 C15 128.9(2) . . ?
C15 C3 Ce1 128.26(15) . . ?
C2 C3 Ce1 79.57(13) . . ?
C2 C3 C8 106.0(2) . . ?
C2 C3 C15 124.4(2) . . ?
C20 C15 C3 121.8(2) . . ?
C16 C15 C3 120.4(2) . . ?
C16 C15 C20 117.7(2) . . ?
Ce1 C2 H2 124.0 . . ?
C3 C2 Ce1 72.25(12) . . ?
C3 C2 H2 123.9 . . ?
C3 C2 C1 112.2(2) . . ?
C1 C2 Ce1 71.39(12) . . ?
C1 C2 H2 123.9 . . ?
C21 C22 H22 119.6 . . ?
C23 C22 C21 120.7(3) . . ?
C23 C22 H22 119.6 . . ?
C15 C20 H20 119.6 . . ?
C19 C20 C15 120.9(3) . . ?
C19 C20 H20 119.6 . . ?
C27 C6 Ce1 114.07(15) . . ?
C5 C6 Ce1 82.12(13) . . ?
C5 C6 C27 124.5(2) . . ?
C5 C6 C7 106.0(2) . . ?
C7 C6 Ce1 65.60(12) . . ?
C7 C6 C27 129.4(2) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 C10 120.6(3) . . ?
C12 C11 H11 119.7 . . ?
C21 C26 H26 119.2 . . ?
C25 C26 C21 121.5(2) . . ?
C25 C26 H26 119.2 . . ?
C8 C7 Ce1 74.01(13) . . ?
C8 C7 C1 107.85(19) . . ?
C6 C7 Ce1 83.25(13) . . ?
C6 C7 C8 108.1(2) . . ?
C6 C7 C1 137.1(2) . . ?
C1 C7 Ce1 84.84(13) . . ?
C9 C1 Ce1 131.44(15) . . ?
C2 C1 Ce1 80.09(12) . . ?
C2 C1 C9 122.7(2) . . ?
C2 C1 C7 105.7(2) . . ?
C7 C1 Ce1 64.17(12) . . ?
C7 C1 C9 130.1(2) . . ?
C9 C14 H14 119.3 . . ?
C13 C14 C9 121.3(3) . . ?
C13 C14 H14 119.3 . . ?
C27 C28 H28 119.2 . . ?
C29 C28 C27 121.5(2) . . ?
C29 C28 H28 119.2 . . ?
C22 C23 H23 119.7 . . ?
C24 C23 C22 120.6(3) . . ?
C24 C23 H23 119.7 . . ?
C20 C19 H19 119.8 . . ?
C20 C19 C18 120.4(3) . . ?
C18 C19 H19 119.8 . . ?
C27 C32 H32 119.5 . . ?
C31 C32 C27 120.9(3) . . ?
C31 C32 H32 119.5 . . ?
C14 C13 H13 119.8 . . ?
C12 C13 C14 120.3(3) . . ?
C12 C13 H13 119.8 . . ?
C15 C16 H16 119.3 . . ?
C17 C16 C15 121.4(3) . . ?
C17 C16 H16 119.3 . . ?
C26 C25 H25 120.0 . . ?
C24 C25 C26 120.0(3) . . ?
C24 C25 H25 120.0 . . ?
C32 C31 H31 119.6 . . ?
C30 C31 C32 120.7(3) . . ?
C30 C31 H31 119.6 . . ?
C23 C24 H24 120.2 . . ?
C25 C24 C23 119.5(3) . . ?
C25 C24 H24 120.2 . . ?
C16 C17 H17 120.0 . . ?
C18 C17 C16 120.0(3) . . ?
C18 C17 H17 120.0 . . ?
C28 C29 H29 120.0 . . ?
C30 C29 C28 119.9(3) . . ?
C30 C29 H29 120.0 . . ?
C31 C30 C29 119.4(3) . . ?
C31 C30 H30 120.3 . . ?
C29 C30 H30 120.3 . . ?
C19 C18 H18 120.2 . . ?
C17 C18 C19 119.6(3) . . ?
C17 C18 H18 120.2 . . ?
C11 C12 H12 120.3 . . ?
C13 C12 C11 119.3(2) . . ?
C13 C12 H12 120.3 . . ?
O1 C34 H34A 109.9 . . ?
O1 C34 H34B 109.9 . . ?
O1 C34 C35 109.0(3) . . ?
H34A C34 H34B 108.3 . . ?
C35 C34 H34A 109.9 . . ?
C35 C34 H34B 109.9 . . ?
O4 C40 H40A 109.5 . . ?
O4 C40 H40B 109.5 . . ?
O4 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
O2 C35 C34 110.2(3) . . ?
O2 C35 H35A 109.6 . . ?
O2 C35 H35B 109.6 . . ?
C34 C35 H35A 109.6 . . ?
C34 C35 H35B 109.6 . . ?
H35A C35 H35B 108.1 . . ?
O1 C33 H33A 109.5 . . ?
O1 C33 H33B 109.5 . . ?
O1 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O2 C36 H36A 109.5 . . ?
O2 C36 H36B 109.5 . . ?
O2 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O3 C37 H37A 109.5 . . ?
O3 C37 H37B 109.5 . . ?
O3 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O4 C39 H39A 109.6 . . ?
O4 C39 H39B 109.6 . . ?
O4 C39 C38 110.2(4) . . ?
H39A C39 H39B 108.1 . . ?
C38 C39 H39A 109.6 . . ?
C38 C39 H39B 109.6 . . ?
O3 C38 C39 110.9(3) . . ?
O3 C38 H38A 109.5 . . ?
O3 C38 H38B 109.5 . . ?
C39 C38 H38A 109.5 . . ?
C39 C38 H38B 109.5 . . ?
H38A C38 H38B 108.0 . . ?
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 C4 2.829(2) . ?
Ce1 C4 2.829(2) 2 ?
Ce1 C8 2.561(2) 2 ?
Ce1 C8 2.561(2) . ?
Ce1 C3 2.839(2) 2 ?
Ce1 C3 2.839(2) . ?
Ce1 C6 2.779(2) 2 ?
Ce1 C6 2.779(2) . ?
Ce1 C7 2.549(2) 2 ?
Ce1 C7 2.549(2) . ?
Ce1 C1 2.820(2) 2 ?
Ce1 C1 2.820(2) . ?
K1 O1 2.760(2) 2_655 ?
K1 O1 2.760(2) . ?
K1 O2 2.855(2) 2_655 ?
K1 O2 2.855(2) . ?
K1 O4 2.907(2) . ?
K1 O4 2.907(2) 2_655 ?
K1 O3 2.752(3) . ?
K1 O3 2.752(3) 2_655 ?
O1 C34 1.421(4) . ?
O1 C33 1.411(5) . ?
O2 C35 1.417(4) . ?
O2 C36 1.426(5) . ?
O4 C40 1.409(4) . ?
O4 C39 1.414(5) . ?
O3 C37 1.421(5) . ?
O3 C38 1.388(5) . ?
C9 C10 1.405(3) . ?
C9 C1 1.462(3) . ?
C9 C14 1.404(3) . ?
C4 C21 1.471(3) . ?
C4 C8 1.452(3) . ?
C4 C5 1.418(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.392(4) . ?
C21 C22 1.398(3) . ?
C21 C26 1.403(3) . ?
C8 C3 1.453(3) . ?
C8 C7 1.448(3) . ?
C27 C6 1.474(3) . ?
C27 C28 1.399(4) . ?
C27 C32 1.401(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.414(3) . ?
C3 C15 1.459(3) . ?
C3 C2 1.407(3) . ?
C15 C20 1.408(3) . ?
C15 C16 1.398(4) . ?
C2 H2 0.9500 . ?
C2 C1 1.421(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.394(4) . ?
C20 H20 0.9500 . ?
C20 C19 1.385(4) . ?
C6 C7 1.448(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.390(4) . ?
C26 H26 0.9500 . ?
C26 C25 1.388(4) . ?
C7 C1 1.458(3) . ?
C14 H14 0.9500 . ?
C14 C13 1.389(4) . ?
C28 H28 0.9500 . ?
C28 C29 1.391(4) . ?
C23 H23 0.9500 . ?
C23 C24 1.387(4) . ?
C19 H19 0.9500 . ?
C19 C18 1.389(5) . ?
C32 H32 0.9500 . ?
C32 C31 1.390(4) . ?
C13 H13 0.9500 . ?
C13 C12 1.387(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.388(4) . ?
C25 H25 0.9500 . ?
C25 C24 1.385(4) . ?
C31 H31 0.9500 . ?
C31 C30 1.383(5) . ?
C24 H24 0.9500 . ?
C17 H17 0.9500 . ?
C17 C18 1.387(5) . ?
C29 H29 0.9500 . ?
C29 C30 1.390(4) . ?
C30 H30 0.9500 . ?
C18 H18 0.9500 . ?
C12 H12 0.9500 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.491(6) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 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 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C38 1.493(7) . ?
C38 H38A 0.9900 . ?
C38 H38B 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
Ce1 C4 C21 C22 -143.9(2) . . . . ?
Ce1 C4 C21 C26 33.8(3) . . . . ?
Ce1 C4 C8 C3 -77.2(3) . . . . ?
Ce1 C4 C8 C7 70.31(15) . . . . ?
Ce1 C4 C5 C6 -57.59(17) . . . . ?
Ce1 C8 C3 C15 -119.5(2) . . . . ?
Ce1 C8 C3 C2 69.55(16) . . . . ?
Ce1 C8 C7 C6 77.16(16) . . . . ?
Ce1 C8 C7 C1 -79.01(16) . . . . ?
Ce1 C5 C6 C27 113.9(2) . . . . ?
Ce1 C5 C6 C7 -61.74(15) . . . . ?
Ce1 C3 C15 C20 76.5(3) . . . . ?
Ce1 C3 C15 C16 -106.7(2) . . . . ?
Ce1 C3 C2 C1 60.47(16) . . . . ?
Ce1 C2 C1 C9 -133.4(2) . . . . ?
Ce1 C2 C1 C7 59.44(14) . . . . ?
Ce1 C6 C7 C8 -70.70(15) . . . . ?
Ce1 C6 C7 C1 74.9(3) . . . . ?
Ce1 C7 C1 C9 123.6(2) . . . . ?
Ce1 C7 C1 C2 -70.47(16) . . . . ?
K1 O1 C34 C35 48.2(3) . . . . ?
K1 O2 C35 C34 44.9(4) . . . . ?
K1 O4 C39 C38 56.9(4) . . . . ?
K1 O3 C38 C39 28.3(6) . . . . ?
O1 C34 C35 O2 -61.3(4) . . . . ?
O4 C39 C38 O3 -58.2(6) . . . . ?
C9 C10 C11 C12 0.1(4) . . . . ?
C9 C14 C13 C12 0.4(4) . . . . ?
C4 C21 C22 C23 178.7(3) . . . . ?
C4 C21 C26 C25 -177.7(2) . . . . ?
C4 C8 C3 Ce1 77.1(3) . . . . ?
C4 C8 C3 C15 -42.4(4) . . . . ?
C4 C8 C3 C2 146.6(3) . . . . ?
C4 C8 C7 Ce1 -78.59(16) . . . . ?
C4 C8 C7 C6 -1.4(3) . . . . ?
C4 C8 C7 C1 -157.60(19) . . . . ?
C4 C5 C6 Ce1 58.73(17) . . . . ?
C4 C5 C6 C27 172.6(2) . . . . ?
C4 C5 C6 C7 -3.0(3) . . . . ?
C10 C9 C1 Ce1 -69.0(3) . . . . ?
C10 C9 C1 C2 38.1(3) . . . . ?
C10 C9 C1 C7 -158.1(2) . . . . ?
C10 C9 C14 C13 -0.6(4) . . . . ?
C10 C11 C12 C13 -0.4(4) . . . . ?
C21 C4 C8 Ce1 108.6(2) . . . . ?
C21 C4 C8 C3 31.4(4) . . . . ?
C21 C4 C8 C7 178.9(2) . . . . ?
C21 C4 C5 Ce1 -119.6(2) . . . . ?
C21 C4 C5 C6 -177.2(2) . . . . ?
C21 C22 C23 C24 -1.1(5) . . . . ?
C21 C26 C25 C24 -1.0(4) . . . . ?
C8 C4 C21 C22 135.8(3) . . . . ?
C8 C4 C21 C26 -46.6(4) . . . . ?
C8 C4 C5 Ce1 59.72(14) . . . . ?
C8 C4 C5 C6 2.1(3) . . . . ?
C8 C3 C15 C20 162.0(2) . . . . ?
C8 C3 C15 C16 -21.3(4) . . . . ?
C8 C3 C2 Ce1 -58.94(14) . . . . ?
C8 C3 C2 C1 1.5(3) . . . . ?
C8 C7 C1 Ce1 71.36(15) . . . . ?
C8 C7 C1 C9 -165.0(2) . . . . ?
C8 C7 C1 C2 0.9(2) . . . . ?
C27 C6 C7 Ce1 -102.0(2) . . . . ?
C27 C6 C7 C8 -172.7(2) . . . . ?
C27 C6 C7 C1 -27.0(4) . . . . ?
C27 C28 C29 C30 1.0(4) . . . . ?
C27 C32 C31 C30 1.2(4) . . . . ?
C5 C4 C21 C22 -45.0(3) . . . . ?
C5 C4 C21 C26 132.6(3) . . . . ?
C5 C4 C8 Ce1 -70.68(16) . . . . ?
C5 C4 C8 C3 -147.9(3) . . . . ?
C5 C4 C8 C7 -0.4(2) . . . . ?
C5 C6 C7 Ce1 73.35(16) . . . . ?
C5 C6 C7 C8 2.7(3) . . . . ?
C5 C6 C7 C1 148.3(3) . . . . ?
C3 C8 C7 Ce1 79.02(16) . . . . ?
C3 C8 C7 C6 156.18(19) . . . . ?
C3 C8 C7 C1 0.0(2) . . . . ?
C3 C15 C20 C19 177.0(2) . . . . ?
C3 C15 C16 C17 -177.4(3) . . . . ?
C3 C2 C1 Ce1 -60.97(17) . . . . ?
C3 C2 C1 C9 165.7(2) . . . . ?
C3 C2 C1 C7 -1.5(3) . . . . ?
C15 C3 C2 Ce1 129.6(2) . . . . ?
C15 C3 C2 C1 -170.0(2) . . . . ?
C15 C20 C19 C18 0.4(4) . . . . ?
C15 C16 C17 C18 0.3(5) . . . . ?
C2 C3 C15 C20 -28.5(3) . . . . ?
C2 C3 C15 C16 148.2(2) . . . . ?
C22 C21 C26 C25 0.0(4) . . . . ?
C22 C23 C24 C25 0.2(5) . . . . ?
C20 C15 C16 C17 -0.6(4) . . . . ?
C20 C19 C18 C17 -0.7(5) . . . . ?
C6 C27 C28 C29 177.3(2) . . . . ?
C6 C27 C32 C31 -178.5(2) . . . . ?
C6 C7 C1 Ce1 -74.3(3) . . . . ?
C6 C7 C1 C9 49.3(4) . . . . ?
C6 C7 C1 C2 -144.8(3) . . . . ?
C26 C21 C22 C23 1.0(4) . . . . ?
C26 C25 C24 C23 0.8(5) . . . . ?
C7 C8 C3 Ce1 -70.45(15) . . . . ?
C7 C8 C3 C15 170.1(2) . . . . ?
C7 C8 C3 C2 -0.9(2) . . . . ?
C1 C9 C10 C11 -176.1(2) . . . . ?
C1 C9 C14 C13 175.9(2) . . . . ?
C14 C9 C10 C11 0.4(3) . . . . ?
C14 C9 C1 Ce1 114.5(2) . . . . ?
C14 C9 C1 C2 -138.3(2) . . . . ?
C14 C9 C1 C7 25.5(4) . . . . ?
C14 C13 C12 C11 0.1(4) . . . . ?
C28 C27 C6 Ce1 -46.3(3) . . . . ?
C28 C27 C6 C5 -143.4(2) . . . . ?
C28 C27 C6 C7 31.1(4) . . . . ?
C28 C27 C32 C31 -1.6(4) . . . . ?
C28 C29 C30 C31 -1.4(4) . . . . ?
C32 C27 C6 Ce1 130.5(2) . . . . ?
C32 C27 C6 C5 33.3(3) . . . . ?
C32 C27 C6 C7 -152.1(2) . . . . ?
C32 C27 C28 C29 0.5(4) . . . . ?
C32 C31 C30 C29 0.3(4) . . . . ?
C16 C15 C20 C19 0.2(4) . . . . ?
C16 C17 C18 C19 0.4(5) . . . . ?
C40 O4 C39 C38 -168.5(4) . . . . ?
C33 O1 C34 C35 -167.4(3) . . . . ?
C36 O2 C35 C34 -178.1(3) . . . . ?
C37 O3 C38 C39 -176.3(4) . . . . ?
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
1.0002 -0.0013 -2.0025 0.0350 0.1581 0.0462
-1.0002 0.0013 2.0025 -0.0350 -0.1581 -0.0462
1.0010 -0.0010 0.0010 0.0879 0.0242 0.0347
-1.0010 0.0010 -0.0010 -0.0879 -0.0242 -0.0347
2.0049 0.9971 0.0011 0.1289 0.0176 0.2098
2.0082 1.9963 1.0019 0.1084 -0.0800 0.3445
-1.0064 -1.9969 1.0027 0.0324 -0.0297 -0.3213
2.0024 -0.0017 1.0038 0.2022 -0.0186 0.0636
0.0062 1.9983 0.9998 -0.0674 -0.1284 0.2751
-1.0014 0.0008 -1.0028 -0.1144 0.0428 -0.0289
