#------------------------------------------------------------------------------
#$Date: 2024-10-06 09:25:44 +0300 (Sun, 06 Oct 2024) $
#$Revision: 295157 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/33/7133325.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_7133325
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 Tb, C16 H40 K O8'
_chemical_formula_sum            'C80 H84 K O8 Tb'
_chemical_formula_weight         1371.49
_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             2023-09-23
_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                 94.6430(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.62410(10)
_cell_length_b                   10.22140(10)
_cell_length_c                   21.5624(2)
_cell_measurement_reflns_used    48670
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      79.2060
_cell_measurement_theta_min      3.3590
_cell_volume                     3432.22(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.102a (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 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -76.00 -44.00   0.50    1.04    --  -47.94 103.00-139.00   64
  2  ω    -37.00   4.00   0.50    1.04    --  -47.94 103.00-139.00   82
  3  ω    -73.00 -47.00   0.50    4.14    --  -91.75 103.00-139.00   52
  4  ω    118.00 143.00   0.50    4.14    --  113.25 103.00-139.00   50
  5  ω     81.00 107.00   0.50    4.14    --  113.25-103.00 118.00   52
  6  ω     43.00  72.00   0.50    4.14    --  113.25-103.00 118.00   58
  7  ω    -18.00   8.00   0.50    1.04    --   10.00  88.00  46.51   52
  8  ω    -14.00  12.00   0.50    1.04    --   10.00  80.00 165.83   52
  9  ω    -16.00   9.00   0.50    1.04    --   10.00  84.00  92.75   50
 10  ω    -17.00   8.00   0.50    1.04    --   10.00  86.00 -49.47   50
 11  ω     -1.00  24.00   0.50    1.04    --   18.00  67.00-114.64   50
 12  ω      6.00  31.00   0.50    1.04    --   22.00  61.00 -72.88   50
 13  ω     13.00  40.00   0.50    1.04    --   26.00  55.00  -7.68   54
 14  ω     17.00  42.00   0.50    1.04    --   30.00  55.00-144.27   50
 15  ω     18.00  44.00   0.50    1.04    --   30.00  53.00-108.01   52
 16  ω    -55.00 -29.00   0.50    1.04    --  -42.00 -49.00  87.36   52
 17  ω    -10.00  27.00   0.50    1.04    --  -47.94  19.00   0.00   74
 18  ω     -8.00  23.00   0.50    1.04    --  -47.94  19.00 120.00   62
 19  ω    -16.00  25.00   0.50    1.04    --  -47.94  19.00-120.00   82
 20  ω    -22.00   7.00   0.50    1.04    --   47.94 -19.00-180.00   58
 21  ω    -21.00  34.00   0.50    1.04    --   47.94 -37.00-150.00  110
 22  ω     20.00  80.00   0.50    1.04    --   47.94-103.00 118.00  120
 23  ω   -159.00-126.00   0.50    4.14    --  -91.75 -61.00-150.00   66
 24  ω   -163.00-112.00   0.50    4.14    --  -91.75 -77.00 -30.00  102
 25  ω   -157.00-118.00   0.50    4.14    --  -91.75 -61.00-120.00   78
 26  ω    -51.00 -21.00   0.50    4.14    --  -91.75  45.00   0.00   60
 27  ω   -147.00-122.00   0.50    4.14    --  -91.75-103.00 118.00   50
 28  ω    -51.00 -26.00   0.50    4.14    --  -91.75  45.00-180.00   50
 29  ω     81.00 106.00   0.50    4.14    --  113.25 -94.00 -30.00   50
 30  ω    149.00 175.00   0.50    4.14    --  113.25  61.00 -90.00   52
 31  ω     42.00  67.00   0.50    4.14    --  113.25 -61.00 -90.00   50
 32  ω     45.00 110.00   0.50    4.14    --  113.25-125.00 120.00  130
 33  ω     45.00  70.00   0.50    4.14    --  113.25 -61.00-150.00   50
 34  ω     42.00  75.00   0.50    4.14    --  113.25 -94.00 -30.00   66
 35  ω     44.00  70.00   0.50    4.14    --  113.25 -77.00 -30.00   52
 36  ω    108.00 133.00   0.50    4.14    --  113.25  30.00  30.00   50
 37  ω    102.00 149.00   0.50    4.14    --  113.25 125.00 -90.00   94
 38  ω    109.00 146.00   0.50    4.14    --  113.25  61.00 -90.00   74
 39  ω    137.00 163.00   0.50    4.14    --  113.25  15.00   0.00   52
 40  ω    111.00 137.00   0.50    4.14    --  113.25  77.00 -90.00   52
 41  ω     68.00 108.00   0.50    4.14    --  113.25-125.00  90.00   80
 42  ω     96.00 131.00   0.50    4.14    --  113.25 125.00 -30.00   70
 43  ω    102.00 132.00   0.50    4.14    --  113.25  15.00   0.00   60
 44  ω     88.00 114.00   0.50    4.14    --  113.25 -79.00 142.85   52
 45  ω     58.00  84.00   0.50    4.14    --  113.25-125.00-150.00   52
 46  ω     44.00  69.00   0.50    4.14    --  113.25 -61.00  30.00   50
 47  ω     63.00 108.00   0.50    4.14    --  113.25-125.00-180.00   90
 48  ω     74.00 105.00   0.50    4.14    --  113.25 -94.00   0.00   62
 49  ω    140.00 166.00   0.50    4.14    --  113.25 125.00-180.00   52
 50  ω    139.00 165.00   0.50    4.14    --  113.25  30.00 -90.00   52
 51  ω     61.00  91.00   0.50    4.14    --  113.25 -94.00 120.00   60
 52  ω    134.00 167.00   0.50    4.14    --  113.25  15.00 120.00   66
 53  ω     42.00  67.00   0.50    4.14    --  113.25 -61.00 -60.00   50
 54  ω    145.00 170.00   0.50    4.14    --  113.25 125.00 -30.00   50
 55  ω     47.00  75.00   0.50    4.14    --  113.25 -94.00 -60.00   56
 56  ω     79.00 106.00   0.50    4.14    --  113.25 -94.00 -60.00   54
 57  ω     44.00  69.00   0.50    4.14    --  113.25 -77.00 150.00   50
 58  ω     45.00  71.00   0.50    4.14    --  113.25 -94.00   0.00   52
 59  ω    128.00 177.00   0.50    4.14    --  113.25  77.00 120.00   98
 60  ω     50.00  75.00   0.50    4.14    --  113.25 -77.00  30.00   50
 61  ω    101.00 133.00   0.50    4.14    --  113.25 -77.00  30.00   64
 62  ω     56.00 106.00   0.50    4.14    --  113.25-125.00  30.00  100
 63  ω    131.00 171.00   0.50    4.14    --  113.25 125.00 -60.00   80
 64  ω     45.00  70.00   0.50    4.14    --  113.25 -61.00-120.00   50
 65  ω     66.00 118.00   0.50    4.14    --  113.25 -83.00-141.43  104
 66  ω     76.00 102.00   0.50    4.14    --  113.25 -77.00 -30.00   52
 67  ω    102.00 144.00   0.50    4.14    --  113.25  45.00  30.00   84
 68  ω     95.00 161.00   0.50    4.14    --  113.25 125.00  60.00  132
 69  ω     44.00  69.00   0.50    4.14    --  113.25 -61.00   0.00   50
 70  ω    148.00 173.00   0.50    4.14    --  113.25  30.00-150.00   50
 71  ω     65.00 105.00   0.50    4.14    --  113.25 -94.00 -90.00   80
 72  ω    122.00 172.00   0.50    4.14    --  113.25  77.00  30.00  100
 73  ω    121.00 146.00   0.50    4.14    --  113.25  45.00 -60.00   50
 74  ω    141.00 167.00   0.50    4.14    --  113.25  61.00 150.00   52
 75  ω    109.00 134.00   0.50    4.14    --  113.25  61.00 150.00   50
 76  ω     44.00  71.00   0.50    4.14    --  113.25 -61.00  90.00   54
 77  ω     43.00  70.00   0.50    4.14    --  113.25 -61.00 120.00   54
 78  ω    135.00 172.00   0.50    4.14    --  113.25  61.00   0.00   74
 79  ω     64.00  90.00   0.50    4.14    --  113.25 -77.00 120.00   52
 80  ω    103.00 132.00   0.50    4.14    --  113.25 -77.00 120.00   58
 81  ω    102.00 143.00   0.50    4.14    --  113.25  45.00  60.00   82
 82  ω    109.00 138.00   0.50    4.14    --  113.25  30.00-150.00   58
 83  ω    110.00 141.00   0.50    4.14    --  113.25  61.00-120.00   62
 84  ω     50.00  76.00   0.50    4.14    --  113.25 -94.00  90.00   52
 85  ω     80.00 106.00   0.50    4.14    --  113.25 -94.00 150.00   52
 86  ω     42.00  68.00   0.50    4.14    --  113.25 -94.00 150.00   52
 87  ω    104.00 130.00   0.50    4.14    --  113.25  30.00 120.00   52
 88  ω    147.00 173.00   0.50    4.14    --  113.25  30.00 120.00   52
 89  ω     53.00 106.00   0.50    4.14    --  113.25 -94.00-150.00  106
 90  ω     96.00 158.00   0.50    4.14    --  113.25 125.00 120.00  124
 91  ω     56.00  82.00   0.50    4.14    --  113.25 -94.00-120.00   52
 92  ω    111.00 174.00   0.50    4.14    --  113.25  77.00-120.00  126
 93  ω    141.00 167.00   0.50    4.14    --  113.25  61.00-180.00   52
 94  ω    106.00 178.00   0.50    4.14    --  113.25  61.00  60.00  144
 95  ω     58.00 101.00   0.50    4.14    --  113.25 -94.00  30.00   86
 96  ω     95.00 122.00   0.50    4.14    --  113.25 -77.00-120.00   54
 97  ω     81.00 106.00   0.50    4.14    --  113.25 -94.00  60.00   50
 98  ω    102.00 131.00   0.50    4.14    --  113.25  45.00 -30.00   58
 99  ω     67.00  93.00   0.50    4.14    --  113.25-125.00-120.00   52
100  ω     80.00 110.00   0.50    4.14    --  113.25-125.00   0.00   60
101  ω     42.00  70.00   0.50    4.14    --  113.25 -61.00-180.00   56
102  ω    147.00 176.00   0.50    4.14    --  113.25  30.00  30.00   58
103  ω    109.00 146.00   0.50    4.14    --  113.25  61.00-150.00   74
104  ω    133.00 170.00   0.50    4.14    --  113.25  15.00-180.00   74
105  ω    131.00 157.00   0.50    4.14    --  113.25  15.00  90.00   52
106  ω    115.00 141.00   0.50    4.14    --  113.25  45.00-120.00   52
107  ω    108.00 134.00   0.50    4.14    --  113.25  30.00-120.00   52
108  ω    134.00 160.00   0.50    4.14    --  113.25  30.00 150.00   52
109  ω     44.00  70.00   0.50    4.14    --  113.25 -61.00 150.00   52
110  ω    100.00 135.00   0.50    4.14    --  113.25 -76.00 -33.43   70
111  ω     42.00  68.00   0.50    4.14    --  113.25 -61.00 -30.00   52
;
_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      0.0271346000
_diffrn_orient_matrix_UB_12      -0.0393642000
_diffrn_orient_matrix_UB_13      0.0676906000
_diffrn_orient_matrix_UB_21      0.0951044000
_diffrn_orient_matrix_UB_22      0.0159536000
_diffrn_orient_matrix_UB_23      -0.0126746000
_diffrn_orient_matrix_UB_31      -0.0031014000
_diffrn_orient_matrix_UB_32      0.1446083000
_diffrn_orient_matrix_UB_33      0.0198260000
_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  0.0700
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_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            82493
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.191
_diffrn_reflns_theta_min         3.367
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.047
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.676
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.102a (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_density_diffrn    1.327
_exptl_crystal_description       plate
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         7466
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0386P)²+3.4342P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.0827
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7273
_reflns_number_total             7466
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4cc02570a2.cif
_cod_data_source_block           pla23115_refinalized
_cod_depositor_comments
'Adding full bibliography for 7133320--7133330.cif.'
_cod_database_code               7133325
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Tb C80 H64 K O8'
_chemical_oxdiff_usercomment     NJK-07-073
_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   0.752
_shelx_estimated_absorpt_t_min   0.393
_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:
 C35(H35A,H35B), C34(H34A,H34B), C39(H39A,H39B), C38(H38A,H38B)
2.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C2(H2), C32(H32), C26(H26), C5(H5), C22(H22), C28(H28), C16(H16),
 C10(H10), C11(H11), C23(H23), C31(H31), C25(H25), C19(H19), C24(H24), C14(H14),
  C17(H17), C18(H18), C29(H29), C13(H13), C30(H30), C12(H12)
2.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C36(H36A,H36B,H36C), C33(H33A,H33B,H33C), 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 3.663
_oxdiff_exptl_absorpt_empirical_full_min 0.545
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
Tb1 Tb 0.750000 0.58371(2) 0.750000 0.01918(6) Uani 1 2 d S T P . .
K1 K 0.250000 1.07838(7) 0.750000 0.03054(14) Uani 1 2 d S T P . .
O1 O 0.33844(14) 1.2223(3) 0.66019(10) 0.0573(6) Uani 1 1 d . . . . .
O4 O 0.18659(15) 0.9436(2) 0.63573(11) 0.0543(5) Uani 1 1 d . . . . .
O2 O 0.36451(15) 1.2714(2) 0.78786(10) 0.0524(5) Uani 1 1 d . . . . .
O3 O 0.33813(14) 0.8735(3) 0.70409(12) 0.0590(6) Uani 1 1 d . . . . .
C21 C 0.61760(14) 0.3373(2) 0.81592(10) 0.0240(4) Uani 1 1 d . . . . .
C1 C 0.62545(13) 0.7538(2) 0.70252(10) 0.0219(4) Uani 1 1 d . . . . .
C7 C 0.60477(13) 0.6153(2) 0.69924(10) 0.0219(4) Uani 1 1 d . . . . .
C27 C 0.63953(14) 0.4962(2) 0.59459(10) 0.0239(4) Uani 1 1 d . . . . .
C6 C 0.62662(13) 0.5042(2) 0.66147(10) 0.0227(4) Uani 1 1 d . . . . .
C20 C 0.63363(15) 0.7876(2) 0.90855(10) 0.0256(4) Uani 1 1 d . . . . .
H20 H 0.678777 0.838552 0.894048 0.031 Uiso 1 1 calc R U . . .
C15 C 0.59149(14) 0.6951(2) 0.86894(10) 0.0231(4) Uani 1 1 d . . . . .
C2 C 0.63027(13) 0.78738(19) 0.76578(10) 0.0212(4) Uani 1 1 d . . . . .
H2 H 0.643933 0.872574 0.781159 0.025 Uiso 1 1 calc R U . . .
C32 C 0.60013(17) 0.3963(2) 0.55780(11) 0.0308(5) Uani 1 1 d . . . . .
H32 H 0.564008 0.334995 0.576092 0.037 Uiso 1 1 calc R U . . .
C9 C 0.62756(13) 0.8477(2) 0.65172(10) 0.0229(4) Uani 1 1 d . . . . .
C26 C 0.64594(15) 0.3770(2) 0.87634(11) 0.0267(4) Uani 1 1 d . . . . .
H26 H 0.662191 0.465616 0.883598 0.032 Uiso 1 1 calc R U . . .
C5 C 0.62902(14) 0.3941(2) 0.70169(11) 0.0242(4) Uani 1 1 d . . . . .
H5 H 0.639682 0.307114 0.688801 0.029 Uiso 1 1 calc R U . . .
C4 C 0.61362(14) 0.42930(19) 0.76331(10) 0.0228(4) Uani 1 1 d . . . . .
C22 C 0.59519(15) 0.2057(2) 0.80701(12) 0.0291(5) Uani 1 1 d . . . . .
H22 H 0.577197 0.175580 0.766356 0.035 Uiso 1 1 calc R U . . .
C28 C 0.69299(16) 0.5831(2) 0.56582(11) 0.0277(5) Uani 1 1 d . . . . .
H28 H 0.720363 0.651733 0.589634 0.033 Uiso 1 1 calc R U . . .
C16 C 0.52488(15) 0.6228(2) 0.89184(11) 0.0291(5) Uani 1 1 d . . . . .
H16 H 0.495256 0.559664 0.865882 0.035 Uiso 1 1 calc R U . . .
C8 C 0.59635(13) 0.56870(19) 0.76207(10) 0.0212(4) Uani 1 1 d . . . . .
C3 C 0.61235(13) 0.67923(19) 0.80438(10) 0.0218(4) Uani 1 1 d . . . . .
C10 C 0.67111(14) 0.9681(2) 0.65928(11) 0.0262(4) Uani 1 1 d . . . . .
H10 H 0.702161 0.987715 0.697868 0.031 Uiso 1 1 calc R U . . .
C11 C 0.66929(17) 1.0586(2) 0.61109(12) 0.0326(5) Uani 1 1 d . . . . .
H11 H 0.698902 1.139342 0.617074 0.039 Uiso 1 1 calc R U . . .
C23 C 0.59877(17) 0.1184(2) 0.85646(13) 0.0344(5) Uani 1 1 d . . . . .
H23 H 0.582225 0.029882 0.849443 0.041 Uiso 1 1 calc R U . . .
C31 C 0.61326(19) 0.3858(2) 0.49495(12) 0.0375(6) Uani 1 1 d . . . . .
H31 H 0.585437 0.318351 0.470629 0.045 Uiso 1 1 calc R U . . .
C25 C 0.65078(17) 0.2894(2) 0.92593(11) 0.0328(5) Uani 1 1 d . . . . .
H25 H 0.670733 0.318275 0.966421 0.039 Uiso 1 1 calc R U . . .
C19 C 0.61016(16) 0.8056(2) 0.96882(11) 0.0305(5) Uani 1 1 d . . . . .
H19 H 0.639739 0.868120 0.995169 0.037 Uiso 1 1 calc R U . . .
C24 C 0.62642(18) 0.1597(2) 0.91623(12) 0.0361(6) Uani 1 1 d . . . . .
H24 H 0.628638 0.099962 0.950061 0.043 Uiso 1 1 calc R U . . .
C14 C 0.58190(16) 0.8237(2) 0.59439(11) 0.0299(5) Uani 1 1 d . . . . .
H14 H 0.551259 0.743839 0.588231 0.036 Uiso 1 1 calc R U . . .
C17 C 0.50130(16) 0.6420(2) 0.95209(12) 0.0340(5) Uani 1 1 d . . . . .
H17 H 0.455660 0.592292 0.966720 0.041 Uiso 1 1 calc R U . . .
C18 C 0.54394(17) 0.7330(2) 0.99080(11) 0.0350(5) Uani 1 1 d . . . . .
H18 H 0.528027 0.745669 1.031979 0.042 Uiso 1 1 calc R U . . .
C29 C 0.70700(19) 0.5716(2) 0.50328(12) 0.0350(5) Uani 1 1 d . . . . .
H29 H 0.744214 0.631149 0.484935 0.042 Uiso 1 1 calc R U . . .
C13 C 0.5804(2) 0.9143(2) 0.54622(12) 0.0405(6) Uani 1 1 d . . . . .
H13 H 0.549117 0.895780 0.507603 0.049 Uiso 1 1 calc R U . . .
C30 C 0.6667(2) 0.4731(3) 0.46757(12) 0.0402(6) Uani 1 1 d . . . . .
H30 H 0.675589 0.465567 0.424656 0.048 Uiso 1 1 calc R U . . .
C12 C 0.6246(2) 1.0318(3) 0.55435(13) 0.0421(6) Uani 1 1 d . . . . .
H12 H 0.624169 1.093345 0.521294 0.051 Uiso 1 1 calc R U . . .
C40 C 0.1005(2) 0.9531(4) 0.61203(17) 0.0570(8) Uani 1 1 d . . . . .
H40A H 0.064967 0.896158 0.636027 0.085 Uiso 1 1 calc R U . . .
H40B H 0.095232 0.925967 0.568297 0.085 Uiso 1 1 calc R U . . .
H40C H 0.081022 1.043841 0.615222 0.085 Uiso 1 1 calc R U . . .
C35 C 0.3862(2) 1.3655(3) 0.74316(17) 0.0563(9) Uani 1 1 d . . . . .
H35A H 0.435464 1.418792 0.760331 0.068 Uiso 1 1 calc R U . . .
H35B H 0.336901 1.424740 0.733032 0.068 Uiso 1 1 calc R U . . .
C34 C 0.4089(2) 1.2969(4) 0.68603(17) 0.0611(9) Uani 1 1 d . . . . .
H34A H 0.425541 1.361795 0.655144 0.073 Uiso 1 1 calc R U . . .
H34B H 0.458568 1.238473 0.696313 0.073 Uiso 1 1 calc R U . . .
C36 C 0.3619(3) 1.3278(4) 0.84717(17) 0.0656(10) Uani 1 1 d . . . . .
H36A H 0.322432 1.402442 0.844659 0.098 Uiso 1 1 calc R U . . .
H36B H 0.419532 1.357596 0.862127 0.098 Uiso 1 1 calc R U . . .
H36C H 0.341955 1.262606 0.876063 0.098 Uiso 1 1 calc R U . . .
C33 C 0.3576(3) 1.1585(5) 0.60468(17) 0.0708(11) Uani 1 1 d . . . . .
H33A H 0.405997 1.098631 0.613655 0.106 Uiso 1 1 calc R U . . .
H33B H 0.372733 1.223791 0.574139 0.106 Uiso 1 1 calc R U . . .
H33C H 0.307271 1.108918 0.587847 0.106 Uiso 1 1 calc R U . . .
C39 C 0.2159(3) 0.8126(4) 0.6381(2) 0.0709(11) Uani 1 1 d . . . . .
H39A H 0.197937 0.768108 0.598332 0.085 Uiso 1 1 calc R U . . .
H39B H 0.189863 0.765460 0.671978 0.085 Uiso 1 1 calc R U . . .
C37 C 0.4281(2) 0.8651(5) 0.7186(2) 0.0766(12) Uani 1 1 d . . . . .
H37A H 0.457911 0.898855 0.683730 0.115 Uiso 1 1 calc R U . . .
H37B H 0.444255 0.773524 0.726304 0.115 Uiso 1 1 calc R U . . .
H37C H 0.444188 0.917035 0.755972 0.115 Uiso 1 1 calc R U . . .
C38 C 0.3114(3) 0.8091(5) 0.6491(2) 0.0807(13) Uani 1 1 d . . . . .
H38A H 0.331195 0.717108 0.651466 0.097 Uiso 1 1 calc R U . . .
H38B H 0.337410 0.851528 0.613819 0.097 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'
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'
Tb Tb -9.1472 9.1891 '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 0.0078
1 0 2 0.0438
-1 2 0 0.0783
1 -2 0 0.0941
-1 -1 1 0.0574
1 -2 -2 0.1014
1 1 -1 0.1101
-1 0 1 0.0069
1 0 0 0.0475
-1 0 0 0.0019
-1 0 2 0.0118
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
C1 Tb1 C1 101.39(9) 2_656 . ?
C7 Tb1 C1 133.10(7) . 2_656 ?
C7 Tb1 C1 31.81(6) . . ?
C7 Tb1 C1 31.81(6) 2_656 2_656 ?
C7 Tb1 C1 133.10(7) 2_656 . ?
C7 Tb1 C7 164.90(9) . 2_656 ?
C7 Tb1 C6 157.79(7) . 2_656 ?
C7 Tb1 C6 32.07(6) . . ?
C7 Tb1 C6 157.79(7) 2_656 . ?
C7 Tb1 C6 32.07(6) 2_656 2_656 ?
C7 Tb1 C4 54.08(7) . . ?
C7 Tb1 C4 137.82(7) . 2_656 ?
C7 Tb1 C4 137.82(7) 2_656 . ?
C7 Tb1 C4 54.08(7) 2_656 2_656 ?
C7 Tb1 C3 119.69(7) . 2_656 ?
C7 Tb1 C3 119.70(7) 2_656 . ?
C7 Tb1 C3 53.85(7) 2_656 2_656 ?
C7 Tb1 C3 53.85(7) . . ?
C6 Tb1 C1 152.89(6) . 2_656 ?
C6 Tb1 C1 152.89(6) 2_656 . ?
C6 Tb1 C1 59.20(6) . . ?
C6 Tb1 C1 59.20(6) 2_656 2_656 ?
C6 Tb1 C6 145.28(9) . 2_656 ?
C4 Tb1 C1 82.39(6) 2_656 2_656 ?
C4 Tb1 C1 151.28(6) 2_656 . ?
C4 Tb1 C1 82.39(6) . . ?
C4 Tb1 C1 151.28(6) . 2_656 ?
C4 Tb1 C6 105.79(6) . 2_656 ?
C4 Tb1 C6 105.79(6) 2_656 . ?
C4 Tb1 C6 51.47(6) 2_656 2_656 ?
C4 Tb1 C6 51.47(6) . . ?
C4 Tb1 C4 108.01(9) . 2_656 ?
C4 Tb1 C3 157.09(6) . 2_656 ?
C4 Tb1 C3 60.12(6) 2_656 2_656 ?
C4 Tb1 C3 60.12(6) . . ?
C4 Tb1 C3 157.09(6) 2_656 . ?
C8 Tb1 C1 132.36(6) . 2_656 ?
C8 Tb1 C1 53.55(6) . . ?
C8 Tb1 C1 132.36(6) 2_656 . ?
C8 Tb1 C1 53.55(6) 2_656 2_656 ?
C8 Tb1 C7 34.48(7) . . ?
C8 Tb1 C7 147.23(7) . 2_656 ?
C8 Tb1 C7 34.48(7) 2_656 2_656 ?
C8 Tb1 C7 147.23(7) 2_656 . ?
C8 Tb1 C6 53.83(7) . . ?
C8 Tb1 C6 123.55(7) . 2_656 ?
C8 Tb1 C6 53.83(7) 2_656 2_656 ?
C8 Tb1 C6 123.55(7) 2_656 . ?
C8 Tb1 C4 32.42(6) 2_656 2_656 ?
C8 Tb1 C4 140.38(7) 2_656 . ?
C8 Tb1 C4 140.38(7) . 2_656 ?
C8 Tb1 C4 32.42(6) . . ?
C8 Tb1 C8 172.79(9) 2_656 . ?
C8 Tb1 C3 152.84(7) . 2_656 ?
C8 Tb1 C3 32.39(6) 2_656 2_656 ?
C8 Tb1 C3 32.39(6) . . ?
C8 Tb1 C3 152.84(7) 2_656 . ?
C3 Tb1 C1 100.00(6) 2_656 . ?
C3 Tb1 C1 50.99(6) 2_656 2_656 ?
C3 Tb1 C1 100.00(6) . 2_656 ?
C3 Tb1 C1 50.99(6) . . ?
C3 Tb1 C6 110.19(6) . 2_656 ?
C3 Tb1 C6 82.51(6) . . ?
C3 Tb1 C6 110.19(6) 2_656 . ?
C3 Tb1 C6 82.51(6) 2_656 2_656 ?
C3 Tb1 C3 137.82(9) . 2_656 ?
O1 K1 O1 118.40(11) . 2_556 ?
O1 K1 O4 131.32(7) 2_556 . ?
O1 K1 O4 79.75(7) . . ?
O1 K1 O4 131.32(7) . 2_556 ?
O1 K1 O4 79.75(7) 2_556 2_556 ?
O4 K1 O4 123.80(10) . 2_556 ?
O2 K1 O1 59.65(7) 2_556 2_556 ?
O2 K1 O1 76.63(7) 2_556 . ?
O2 K1 O1 76.63(7) . 2_556 ?
O2 K1 O1 59.65(7) . . ?
O2 K1 O4 85.40(6) . 2_556 ?
O2 K1 O4 139.27(7) . . ?
O2 K1 O4 139.27(7) 2_556 2_556 ?
O2 K1 O4 85.40(6) 2_556 . ?
O2 K1 O2 88.02(10) 2_556 . ?
O3 K1 O1 82.21(8) 2_556 2_556 ?
O3 K1 O1 156.86(8) . 2_556 ?
O3 K1 O1 82.21(8) . . ?
O3 K1 O1 156.86(8) 2_556 . ?
O3 K1 O4 78.36(8) . 2_556 ?
O3 K1 O4 58.71(7) . . ?
O3 K1 O4 58.71(7) 2_556 2_556 ?
O3 K1 O4 78.36(8) 2_556 . ?
O3 K1 O2 141.10(7) 2_556 . ?
O3 K1 O2 141.10(7) . 2_556 ?
O3 K1 O2 108.84(8) 2_556 2_556 ?
O3 K1 O2 108.84(8) . . ?
O3 K1 O3 80.09(12) . 2_556 ?
C34 O1 K1 114.28(18) . . ?
C34 O1 C33 111.7(3) . . ?
C33 O1 K1 118.7(2) . . ?
C40 O4 K1 121.6(2) . . ?
C40 O4 C39 112.1(3) . . ?
C39 O4 K1 109.2(2) . . ?
C35 O2 K1 118.06(18) . . ?
C36 O2 K1 119.96(19) . . ?
C36 O2 C35 111.4(3) . . ?
C37 O3 K1 119.0(2) . . ?
C38 O3 K1 123.1(2) . . ?
C38 O3 C37 112.6(3) . . ?
C26 C21 C4 121.46(19) . . ?
C22 C21 C26 117.6(2) . . ?
C22 C21 C4 120.9(2) . . ?
C7 C1 Tb1 63.19(11) . . ?
C7 C1 C9 128.54(19) . . ?
C2 C1 Tb1 79.13(12) . . ?
C2 C1 C7 106.25(18) . . ?
C2 C1 C9 124.53(19) . . ?
C9 C1 Tb1 129.67(14) . . ?
C1 C7 Tb1 85.00(12) . . ?
C1 C7 C6 136.66(19) . . ?
C6 C7 Tb1 84.06(12) . . ?
C8 C7 Tb1 72.04(12) . . ?
C8 C7 C1 108.12(18) . . ?
C8 C7 C6 108.00(17) . . ?
C32 C27 C6 120.3(2) . . ?
C28 C27 C6 122.16(19) . . ?
C28 C27 C32 117.5(2) . . ?
C7 C6 Tb1 63.87(11) . . ?
C7 C6 C27 130.37(19) . . ?
C27 C6 Tb1 123.83(14) . . ?
C5 C6 Tb1 80.00(13) . . ?
C5 C6 C7 105.85(18) . . ?
C5 C6 C27 123.69(19) . . ?
C15 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
C19 C20 C15 120.8(2) . . ?
C20 C15 C3 121.62(19) . . ?
C16 C15 C20 117.9(2) . . ?
C16 C15 C3 120.4(2) . . ?
Tb1 C2 H2 125.6 . . ?
C1 C2 Tb1 71.83(11) . . ?
C1 C2 H2 123.8 . . ?
C1 C2 C3 112.39(18) . . ?
C3 C2 Tb1 70.34(11) . . ?
C3 C2 H2 123.8 . . ?
C27 C32 H32 119.5 . . ?
C31 C32 C27 120.9(2) . . ?
C31 C32 H32 119.5 . . ?
C10 C9 C1 121.8(2) . . ?
C14 C9 C1 120.5(2) . . ?
C14 C9 C10 117.6(2) . . ?
C21 C26 H26 119.3 . . ?
C25 C26 C21 121.4(2) . . ?
C25 C26 H26 119.3 . . ?
Tb1 C5 H5 128.1 . . ?
C6 C5 Tb1 70.58(12) . . ?
C6 C5 H5 124.0 . . ?
C4 C5 Tb1 68.99(12) . . ?
C4 C5 C6 111.94(18) . . ?
C4 C5 H5 124.0 . . ?
C21 C4 Tb1 118.28(14) . . ?
C5 C4 Tb1 81.53(12) . . ?
C5 C4 C21 124.15(19) . . ?
C5 C4 C8 106.15(18) . . ?
C8 C4 Tb1 64.45(11) . . ?
C8 C4 C21 129.7(2) . . ?
C21 C22 H22 119.4 . . ?
C23 C22 C21 121.2(2) . . ?
C23 C22 H22 119.4 . . ?
C27 C28 H28 119.2 . . ?
C29 C28 C27 121.5(2) . . ?
C29 C28 H28 119.2 . . ?
C15 C16 H16 119.5 . . ?
C17 C16 C15 121.0(2) . . ?
C17 C16 H16 119.5 . . ?
C7 C8 Tb1 73.48(12) . . ?
C7 C8 C3 107.75(17) . . ?
C4 C8 Tb1 83.14(12) . . ?
C4 C8 C7 107.99(18) . . ?
C4 C8 C3 136.6(2) . . ?
C3 C8 Tb1 84.14(12) . . ?
C15 C3 Tb1 134.11(14) . . ?
C2 C3 Tb1 80.02(12) . . ?
C2 C3 C15 122.59(18) . . ?
C2 C3 C8 105.48(18) . . ?
C8 C3 Tb1 63.48(11) . . ?
C8 C3 C15 129.75(18) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 C9 120.9(2) . . ?
C11 C10 H10 119.5 . . ?
C10 C11 H11 119.8 . . ?
C12 C11 C10 120.5(2) . . ?
C12 C11 H11 119.8 . . ?
C22 C23 H23 119.8 . . ?
C22 C23 C24 120.4(2) . . ?
C24 C23 H23 119.8 . . ?
C32 C31 H31 119.8 . . ?
C30 C31 C32 120.4(2) . . ?
C30 C31 H31 119.8 . . ?
C26 C25 H25 120.0 . . ?
C24 C25 C26 120.0(2) . . ?
C24 C25 H25 120.0 . . ?
C20 C19 H19 119.7 . . ?
C18 C19 C20 120.6(2) . . ?
C18 C19 H19 119.7 . . ?
C23 C24 H24 120.4 . . ?
C25 C24 C23 119.3(2) . . ?
C25 C24 H24 120.4 . . ?
C9 C14 H14 119.3 . . ?
C13 C14 C9 121.3(2) . . ?
C13 C14 H14 119.3 . . ?
C16 C17 H17 119.8 . . ?
C18 C17 C16 120.4(2) . . ?
C18 C17 H17 119.8 . . ?
C19 C18 H18 120.4 . . ?
C17 C18 C19 119.3(2) . . ?
C17 C18 H18 120.4 . . ?
C28 C29 H29 120.0 . . ?
C30 C29 C28 120.0(2) . . ?
C30 C29 H29 120.0 . . ?
C14 C13 H13 119.9 . . ?
C12 C13 C14 120.2(3) . . ?
C12 C13 H13 119.9 . . ?
C31 C30 C29 119.5(2) . . ?
C31 C30 H30 120.2 . . ?
C29 C30 H30 120.2 . . ?
C11 C12 C13 119.4(2) . . ?
C11 C12 H12 120.3 . . ?
C13 C12 H12 120.3 . . ?
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 H35A 109.8 . . ?
O2 C35 H35B 109.8 . . ?
O2 C35 C34 109.2(3) . . ?
H35A C35 H35B 108.3 . . ?
C34 C35 H35A 109.8 . . ?
C34 C35 H35B 109.8 . . ?
O1 C34 C35 110.5(3) . . ?
O1 C34 H34A 109.5 . . ?
O1 C34 H34B 109.5 . . ?
C35 C34 H34A 109.5 . . ?
C35 C34 H34B 109.5 . . ?
H34A C34 H34B 108.1 . . ?
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 . . ?
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 . . ?
O4 C39 H39A 109.6 . . ?
O4 C39 H39B 109.6 . . ?
O4 C39 C38 110.1(3) . . ?
H39A C39 H39B 108.1 . . ?
C38 C39 H39A 109.6 . . ?
C38 C39 H39B 109.6 . . ?
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 . . ?
O3 C38 C39 110.6(3) . . ?
O3 C38 H38A 109.5 . . ?
O3 C38 H38B 109.5 . . ?
C39 C38 H38A 109.5 . . ?
C39 C38 H38B 109.5 . . ?
H38A C38 H38B 108.1 . . ?
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
Tb1 C1 2.745(2) . ?
Tb1 C1 2.745(2) 2_656 ?
Tb1 C7 2.460(2) . ?
Tb1 C7 2.460(2) 2_656 ?
Tb1 C6 2.725(2) . ?
Tb1 C6 2.725(2) 2_656 ?
Tb1 C4 2.686(2) 2_656 ?
Tb1 C4 2.686(2) . ?
Tb1 C8 2.440(2) 2_656 ?
Tb1 C8 2.440(2) . ?
Tb1 C3 2.713(2) 2_656 ?
Tb1 C3 2.713(2) . ?
K1 O1 2.874(2) 2_556 ?
K1 O1 2.874(2) . ?
K1 O4 2.925(2) . ?
K1 O4 2.925(2) 2_556 ?
K1 O2 2.743(2) . ?
K1 O2 2.743(2) 2_556 ?
K1 O3 2.735(2) . ?
K1 O3 2.735(2) 2_556 ?
O1 C34 1.415(4) . ?
O1 C33 1.416(4) . ?
O4 C40 1.404(4) . ?
O4 C39 1.415(4) . ?
O2 C35 1.422(4) . ?
O2 C36 1.407(4) . ?
O3 C37 1.417(4) . ?
O3 C38 1.391(5) . ?
C21 C26 1.402(3) . ?
C21 C4 1.471(3) . ?
C21 C22 1.399(3) . ?
C1 C7 1.453(3) . ?
C1 C2 1.402(3) . ?
C1 C9 1.459(3) . ?
C7 C6 1.455(3) . ?
C7 C8 1.452(3) . ?
C27 C6 1.475(3) . ?
C27 C32 1.404(3) . ?
C27 C28 1.399(3) . ?
C6 C5 1.419(3) . ?
C20 H20 0.9500 . ?
C20 C15 1.402(3) . ?
C20 C19 1.391(3) . ?
C15 C16 1.399(3) . ?
C15 C3 1.464(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.425(3) . ?
C32 H32 0.9500 . ?
C32 C31 1.391(4) . ?
C9 C10 1.409(3) . ?
C9 C14 1.398(3) . ?
C26 H26 0.9500 . ?
C26 C25 1.392(3) . ?
C5 H5 0.9500 . ?
C5 C4 1.416(3) . ?
C4 C8 1.450(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.388(3) . ?
C28 H28 0.9500 . ?
C28 C29 1.389(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.393(3) . ?
C8 C3 1.461(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.389(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.386(4) . ?
C23 H23 0.9500 . ?
C23 C24 1.391(4) . ?
C31 H31 0.9500 . ?
C31 C30 1.386(4) . ?
C25 H25 0.9500 . ?
C25 C24 1.390(4) . ?
C19 H19 0.9500 . ?
C19 C18 1.387(4) . ?
C24 H24 0.9500 . ?
C14 H14 0.9500 . ?
C14 C13 1.391(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.384(4) . ?
C18 H18 0.9500 . ?
C29 H29 0.9500 . ?
C29 C30 1.387(4) . ?
C13 H13 0.9500 . ?
C13 C12 1.390(4) . ?
C30 H30 0.9500 . ?
C12 H12 0.9500 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C34 1.485(6) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C38 1.493(6) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
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
Tb1 C1 C7 C6 -75.9(3) . . . . ?
Tb1 C1 C7 C8 69.25(14) . . . . ?
Tb1 C1 C2 C3 -58.79(15) . . . . ?
Tb1 C1 C9 C10 -76.9(2) . . . . ?
Tb1 C1 C9 C14 106.6(2) . . . . ?
Tb1 C7 C6 C27 -113.4(2) . . . . ?
Tb1 C7 C6 C5 70.11(15) . . . . ?
Tb1 C7 C8 C4 -76.86(15) . . . . ?
Tb1 C7 C8 C3 78.06(15) . . . . ?
Tb1 C6 C5 C4 56.51(16) . . . . ?
Tb1 C2 C3 C15 136.6(2) . . . . ?
Tb1 C2 C3 C8 -58.72(13) . . . . ?
Tb1 C5 C4 C21 -118.5(2) . . . . ?
Tb1 C5 C4 C8 60.19(14) . . . . ?
Tb1 C4 C8 C7 70.11(14) . . . . ?
Tb1 C4 C8 C3 -73.9(2) . . . . ?
Tb1 C8 C3 C15 -126.6(2) . . . . ?
Tb1 C8 C3 C2 70.17(15) . . . . ?
K1 O1 C34 C35 -43.3(3) . . . . ?
K1 O4 C39 C38 -55.5(4) . . . . ?
K1 O2 C35 C34 -49.0(3) . . . . ?
K1 O3 C38 C39 -30.1(5) . . . . ?
O4 C39 C38 O3 58.1(5) . . . . ?
O2 C35 C34 O1 60.7(4) . . . . ?
C21 C26 C25 C24 -0.6(4) . . . . ?
C21 C4 C8 Tb1 106.6(2) . . . . ?
C21 C4 C8 C7 176.7(2) . . . . ?
C21 C4 C8 C3 32.7(4) . . . . ?
C21 C22 C23 C24 -1.2(4) . . . . ?
C1 C7 C6 Tb1 76.2(3) . . . . ?
C1 C7 C6 C27 -37.1(4) . . . . ?
C1 C7 C6 C5 146.3(3) . . . . ?
C1 C7 C8 Tb1 -78.32(15) . . . . ?
C1 C7 C8 C4 -155.18(18) . . . . ?
C1 C7 C8 C3 -0.3(2) . . . . ?
C1 C2 C3 Tb1 59.65(16) . . . . ?
C1 C2 C3 C15 -163.78(19) . . . . ?
C1 C2 C3 C8 0.9(2) . . . . ?
C1 C9 C10 C11 -177.2(2) . . . . ?
C1 C9 C14 C13 177.5(2) . . . . ?
C7 C1 C2 Tb1 57.70(14) . . . . ?
C7 C1 C2 C3 -1.1(2) . . . . ?
C7 C1 C9 C10 -161.8(2) . . . . ?
C7 C1 C9 C14 21.7(3) . . . . ?
C7 C6 C5 Tb1 -59.01(14) . . . . ?
C7 C6 C5 C4 -2.5(2) . . . . ?
C7 C8 C3 Tb1 -70.55(14) . . . . ?
C7 C8 C3 C15 162.8(2) . . . . ?
C7 C8 C3 C2 -0.4(2) . . . . ?
C27 C6 C5 Tb1 124.2(2) . . . . ?
C27 C6 C5 C4 -179.3(2) . . . . ?
C27 C32 C31 C30 0.9(4) . . . . ?
C27 C28 C29 C30 0.9(4) . . . . ?
C6 C7 C8 Tb1 77.31(15) . . . . ?
C6 C7 C8 C4 0.5(2) . . . . ?
C6 C7 C8 C3 155.37(18) . . . . ?
C6 C27 C32 C31 -178.6(2) . . . . ?
C6 C27 C28 C29 177.6(2) . . . . ?
C6 C5 C4 Tb1 -57.40(16) . . . . ?
C6 C5 C4 C21 -175.9(2) . . . . ?
C6 C5 C4 C8 2.8(3) . . . . ?
C20 C15 C16 C17 -0.1(3) . . . . ?
C20 C15 C3 Tb1 70.0(3) . . . . ?
C20 C15 C3 C2 -39.4(3) . . . . ?
C20 C15 C3 C8 159.9(2) . . . . ?
C20 C19 C18 C17 0.1(4) . . . . ?
C15 C20 C19 C18 -0.6(3) . . . . ?
C15 C16 C17 C18 -0.4(4) . . . . ?
C2 C1 C7 Tb1 -68.45(15) . . . . ?
C2 C1 C7 C6 -144.3(3) . . . . ?
C2 C1 C7 C8 0.8(2) . . . . ?
C2 C1 C9 C10 28.9(3) . . . . ?
C2 C1 C9 C14 -147.5(2) . . . . ?
C32 C27 C6 Tb1 144.62(18) . . . . ?
C32 C27 C6 C7 -132.6(2) . . . . ?
C32 C27 C6 C5 43.3(3) . . . . ?
C32 C27 C28 C29 -0.1(4) . . . . ?
C32 C31 C30 C29 -0.1(4) . . . . ?
C9 C1 C7 Tb1 120.8(2) . . . . ?
C9 C1 C7 C6 44.9(4) . . . . ?
C9 C1 C7 C8 -170.0(2) . . . . ?
C9 C1 C2 Tb1 -131.1(2) . . . . ?
C9 C1 C2 C3 170.14(19) . . . . ?
C9 C10 C11 C12 -0.2(4) . . . . ?
C9 C14 C13 C12 -0.2(4) . . . . ?
C26 C21 C4 Tb1 47.0(2) . . . . ?
C26 C21 C4 C5 146.4(2) . . . . ?
C26 C21 C4 C8 -32.0(3) . . . . ?
C26 C21 C22 C23 1.6(3) . . . . ?
C26 C25 C24 C23 1.1(4) . . . . ?
C5 C4 C8 Tb1 -72.03(16) . . . . ?
C5 C4 C8 C7 -1.9(2) . . . . ?
C5 C4 C8 C3 -146.0(2) . . . . ?
C4 C21 C26 C25 -179.1(2) . . . . ?
C4 C21 C22 C23 -180.0(2) . . . . ?
C4 C8 C3 Tb1 73.5(3) . . . . ?
C4 C8 C3 C15 -53.1(4) . . . . ?
C4 C8 C3 C2 143.7(2) . . . . ?
C22 C21 C26 C25 -0.7(3) . . . . ?
C22 C21 C4 Tb1 -131.30(18) . . . . ?
C22 C21 C4 C5 -31.9(3) . . . . ?
C22 C21 C4 C8 149.7(2) . . . . ?
C22 C23 C24 C25 -0.2(4) . . . . ?
C28 C27 C6 Tb1 -33.1(3) . . . . ?
C28 C27 C6 C7 49.7(3) . . . . ?
C28 C27 C6 C5 -134.4(2) . . . . ?
C28 C27 C32 C31 -0.8(4) . . . . ?
C28 C29 C30 C31 -0.7(4) . . . . ?
C16 C15 C3 Tb1 -113.7(2) . . . . ?
C16 C15 C3 C2 136.9(2) . . . . ?
C16 C15 C3 C8 -23.8(3) . . . . ?
C16 C17 C18 C19 0.4(4) . . . . ?
C8 C7 C6 Tb1 -68.92(14) . . . . ?
C8 C7 C6 C27 177.7(2) . . . . ?
C8 C7 C6 C5 1.2(2) . . . . ?
C3 C15 C16 C17 -176.5(2) . . . . ?
C10 C9 C14 C13 0.9(3) . . . . ?
C10 C11 C12 C13 0.9(4) . . . . ?
C19 C20 C15 C16 0.6(3) . . . . ?
C19 C20 C15 C3 176.9(2) . . . . ?
C14 C9 C10 C11 -0.7(3) . . . . ?
C14 C13 C12 C11 -0.7(4) . . . . ?
C40 O4 C39 C38 166.8(3) . . . . ?
C36 O2 C35 C34 166.3(3) . . . . ?
C33 O1 C34 C35 178.4(3) . . . . ?
C37 O3 C38 C39 176.0(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
-0.9980 -0.0043 -1.9990 -0.1622 -0.0696 -0.0372
0.9980 0.0043 1.9990 0.1622 0.0696 0.0372
-0.9922 1.9953 -0.0055 -0.1058 -0.0625 0.2915
0.9922 -1.9953 0.0055 0.1058 0.0625 -0.2915
-1.0014 -0.9971 1.0030 0.0800 -0.1239 -0.1212
0.9924 -1.9988 -1.9938 -0.0293 0.0878 -0.3317
1.0014 0.9971 -1.0030 -0.0800 0.1239 0.1212
-0.9984 0.0009 1.0000 0.0406 -0.1076 0.0231
0.9983 0.0008 -0.0003 0.0270 0.0950 -0.0030
-0.9983 -0.0008 0.0003 -0.0270 -0.0950 0.0030
-0.9985 0.0027 1.9997 0.1082 -0.1203 0.0431
