#------------------------------------------------------------------------------
#$Date: 2023-11-16 00:57:39 +0200 (Thu, 16 Nov 2023) $
#$Revision: 287625 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/23/7132351.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_7132351
loop_
_publ_author_name
'Pugliese, Elizabeth R.'
'Benner, Florian'
'Demir, Selvan'
_publ_section_title
;
 Isolation of an organometallic yttrium bismuth cluster and elucidation of
 its electronic structure.
;
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/d3cc04520j
_journal_year                    2023
_chemical_formula_moiety         'C30 H43 O Y'
_chemical_formula_sum            'C30 H43 O Y'
_chemical_formula_weight         508.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-28
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2023-08-31 deposited with the CCDC.	2023-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.699(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4266(2)
_cell_length_b                   17.1628(3)
_cell_length_c                   16.8285(3)
_cell_measurement_reflns_used    16390
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.7180
_cell_measurement_theta_min      3.4140
_cell_volume                     2656.03(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (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(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.821
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -73.00 -46.00   0.50   11.59    --   -4.69 -32.00 132.00   54
  2  ω    -17.00  45.00   0.50   11.59    --   -4.69  32.00 -68.00  124
  3  ω    -26.00   0.00   0.50   11.59    --   -4.69  77.00   0.00   52
  4  ω     12.00  69.00   0.50   11.59    --   -4.69  24.00 -38.60  114
  5  ω    -30.00   5.00   0.50   11.59    --   -4.69 -32.00 132.00   70
  6  ω    -26.00  -1.00   0.50   11.59    --   -4.69  77.00-150.00   50
  7  ω    -15.00  20.00   0.50   11.59    --    5.47 -57.00-120.00   70
  8  ω     -7.00  18.00   0.50   11.59    --    5.47  37.00-150.00   50
  9  ω     13.00  39.00   0.50   11.59    --    5.47 -99.00 120.00   52
 10  ω     40.00  71.00   0.50   11.59    --    5.47   0.00-120.00   62
 11  ω     13.00  39.00   0.50   11.59    --    5.47 -99.00  90.00   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      -0.0097174000
_diffrn_orient_matrix_UB_12      -0.0146980000
_diffrn_orient_matrix_UB_13      0.0378290000
_diffrn_orient_matrix_UB_21      -0.0734152000
_diffrn_orient_matrix_UB_22      -0.0091138000
_diffrn_orient_matrix_UB_23      -0.0180733000
_diffrn_orient_matrix_UB_31      0.0216337000
_diffrn_orient_matrix_UB_32      -0.0375209000
_diffrn_orient_matrix_UB_33      -0.0104560000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.821
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32939
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.821
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.842
_diffrn_reflns_theta_min         2.941
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.214
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.597
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.120a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         6862
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0242P)²+2.4052P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0699
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5975
_reflns_number_total             6862
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3cc04520j2.cif
_cod_data_source_block           erp-ii-124_hex_final
_cod_database_code               7132351
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         YC30H43O
_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   0.705
_shelx_estimated_absorpt_t_min   0.416
_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:
 C27(H27A,H27B), C28(H28A,H28B), C30(H30A,H30B), C29(H29A,H29B)
2.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C25(H25), C22(H22), C23(H23), C24(H24)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C16(H16A,H16B,
 H16C), C6(H6A,H6B,H6C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C7(H7A,H7B,
 H7C), C18(H18A,H18B,H18C), C8(H8A,H8B,H8C)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.775
_oxdiff_exptl_absorpt_empirical_full_min 0.787
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Y1 Y 0.34514(2) 0.55083(2) 0.73016(2) 0.01301(5) Uani 1 1 d . . . . .
O1 O 0.19796(14) 0.43659(7) 0.70030(8) 0.0201(3) Uani 1 1 d . . . . .
C11 C 0.2658(2) 0.52916(10) 0.87185(10) 0.0192(4) Uani 1 1 d . . . . .
C13 C 0.4413(2) 0.62166(10) 0.87306(10) 0.0217(4) Uani 1 1 d . . . . .
C15 C 0.4014(2) 0.49053(10) 0.88247(10) 0.0177(3) Uani 1 1 d . . . . .
C14 C 0.5100(2) 0.54741(11) 0.88328(10) 0.0195(3) Uani 1 1 d . . . . .
C2 C 0.5026(2) 0.61653(10) 0.63281(11) 0.0194(4) Uani 1 1 d . . . . .
C12 C 0.2912(2) 0.61028(10) 0.86714(11) 0.0220(4) Uani 1 1 d . . . . .
C1 C 0.60010(19) 0.56754(10) 0.68637(10) 0.0183(3) Uani 1 1 d . . . . .
C3 C 0.39928(19) 0.56879(11) 0.58107(10) 0.0196(4) Uani 1 1 d . . . . .
C5 C 0.55626(19) 0.48901(10) 0.66861(11) 0.0181(3) Uani 1 1 d . . . . .
C20 C 0.4367(2) 0.40680(10) 0.90648(12) 0.0268(4) Uani 1 1 d . . . . .
H20A H 0.346612 0.378556 0.907153 0.040 Uiso 1 1 calc R U . . .
H20B H 0.500926 0.405056 0.960827 0.040 Uiso 1 1 calc R U . . .
H20C H 0.485455 0.382436 0.867054 0.040 Uiso 1 1 calc R U . . .
C27 C 0.0470(2) 0.43599(10) 0.65593(12) 0.0230(4) Uani 1 1 d . . . . .
H27A H 0.039420 0.450581 0.598233 0.028 Uiso 1 1 calc R U . . .
H27B H -0.011542 0.473011 0.680561 0.028 Uiso 1 1 calc R U . . .
C21 C 0.1565(2) 0.64515(11) 0.66817(11) 0.0237(4) Uani 1 1 d . . . . .
C26 C 0.0198(2) 0.63681(11) 0.61500(12) 0.0243(4) Uani 1 1 d . . . . .
H26 H -0.019476 0.585826 0.605432 0.029 Uiso 1 1 calc R U . . .
C9 C 0.3609(2) 0.42137(13) 0.55488(13) 0.0307(5) Uani 1 1 d . . . . .
H9A H 0.398163 0.373110 0.583013 0.046 Uiso 1 1 calc R U . . .
H9B H 0.381869 0.421767 0.500374 0.046 Uiso 1 1 calc R U . . .
H9C H 0.255547 0.424401 0.550173 0.046 Uiso 1 1 calc R U . . .
C10 C 0.6355(2) 0.41787(11) 0.70787(13) 0.0277(4) Uani 1 1 d . . . . .
H10A H 0.595997 0.402396 0.754743 0.042 Uiso 1 1 calc R U . . .
H10B H 0.739227 0.429745 0.726127 0.042 Uiso 1 1 calc R U . . .
H10C H 0.622753 0.375160 0.668271 0.042 Uiso 1 1 calc R U . . .
C4 C 0.43307(19) 0.49010(10) 0.60256(11) 0.0193(4) Uani 1 1 d . . . . .
C28 C -0.0053(2) 0.35306(11) 0.66237(14) 0.0282(4) Uani 1 1 d . . . . .
H28A H -0.047053 0.346436 0.711014 0.034 Uiso 1 1 calc R U . . .
H28B H -0.079034 0.338210 0.613210 0.034 Uiso 1 1 calc R U . . .
C16 C 0.1205(2) 0.49248(14) 0.87239(12) 0.0310(5) Uani 1 1 d . . . . .
H16A H 0.045139 0.516658 0.830151 0.046 Uiso 1 1 calc R U . . .
H16B H 0.097301 0.500437 0.925777 0.046 Uiso 1 1 calc R U . . .
H16C H 0.124818 0.436518 0.861581 0.046 Uiso 1 1 calc R U . . .
C25 C -0.0614(2) 0.69886(11) 0.57551(12) 0.0249(4) Uani 1 1 d . . . . .
H25 H -0.154260 0.689516 0.541242 0.030 Uiso 1 1 calc R U . . .
C6 C 0.7405(2) 0.59547(13) 0.73963(12) 0.0309(5) Uani 1 1 d . . . . .
H6A H 0.719668 0.634133 0.778369 0.046 Uiso 1 1 calc R U . . .
H6B H 0.800951 0.619222 0.705679 0.046 Uiso 1 1 calc R U . . .
H6C H 0.792362 0.551230 0.769528 0.046 Uiso 1 1 calc R U . . .
C17 C 0.1786(3) 0.67241(13) 0.86806(13) 0.0391(6) Uani 1 1 d . . . . .
H17A H 0.209790 0.721256 0.847044 0.059 Uiso 1 1 calc R U . . .
H17B H 0.167248 0.680302 0.924015 0.059 Uiso 1 1 calc R U . . .
H17C H 0.085400 0.656075 0.833733 0.059 Uiso 1 1 calc R U . . .
C19 C 0.6701(2) 0.53080(14) 0.91029(12) 0.0311(5) Uani 1 1 d . . . . .
H19A H 0.698905 0.492872 0.873240 0.047 Uiso 1 1 calc R U . . .
H19B H 0.690694 0.509545 0.965685 0.047 Uiso 1 1 calc R U . . .
H19C H 0.725049 0.579173 0.909514 0.047 Uiso 1 1 calc R U . . .
C22 C 0.2033(2) 0.72319(12) 0.67809(12) 0.0273(4) Uani 1 1 d . . . . .
H22 H 0.293227 0.733598 0.714869 0.033 Uiso 1 1 calc R U . . .
C7 C 0.5228(3) 0.70288(11) 0.62431(14) 0.0333(5) Uani 1 1 d . . . . .
H7A H 0.432072 0.725936 0.593665 0.050 Uiso 1 1 calc R U . . .
H7B H 0.600595 0.712248 0.595238 0.050 Uiso 1 1 calc R U . . .
H7C H 0.548982 0.726686 0.678498 0.050 Uiso 1 1 calc R U . . .
C30 C 0.2439(2) 0.35695(11) 0.72167(13) 0.0286(4) Uani 1 1 d . . . . .
H30A H 0.248367 0.347116 0.780136 0.034 Uiso 1 1 calc R U . . .
H30B H 0.341205 0.347128 0.710525 0.034 Uiso 1 1 calc R U . . .
C18 C 0.5166(3) 0.69972(12) 0.88051(13) 0.0357(5) Uani 1 1 d . . . . .
H18A H 0.621788 0.691930 0.888842 0.054 Uiso 1 1 calc R U . . .
H18B H 0.495150 0.728164 0.926997 0.054 Uiso 1 1 calc R U . . .
H18C H 0.481614 0.729795 0.830536 0.054 Uiso 1 1 calc R U . . .
C23 C 0.1267(2) 0.78591(12) 0.63763(12) 0.0306(5) Uani 1 1 d . . . . .
H23 H 0.166408 0.836921 0.645467 0.037 Uiso 1 1 calc R U . . .
C29 C 0.1321(2) 0.30565(11) 0.66963(14) 0.0294(4) Uani 1 1 d . . . . .
H29A H 0.124411 0.254893 0.696324 0.035 Uiso 1 1 calc R U . . .
H29B H 0.154610 0.296525 0.615636 0.035 Uiso 1 1 calc R U . . .
C8 C 0.2855(2) 0.59457(14) 0.50879(12) 0.0330(5) Uani 1 1 d . . . . .
H8A H 0.196127 0.564593 0.506385 0.049 Uiso 1 1 calc R U . . .
H8B H 0.320596 0.585806 0.458870 0.049 Uiso 1 1 calc R U . . .
H8C H 0.265318 0.650145 0.513912 0.049 Uiso 1 1 calc R U . . .
C24 C -0.0075(2) 0.77417(11) 0.58592(12) 0.0286(4) Uani 1 1 d . . . . .
H24 H -0.061372 0.816668 0.558246 0.034 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 0.0033 0.0016 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 '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
0 1 1 0.2411
1 0 -2 0.1312
1 1 -2 0.1553
-1 2 2 0.1599
-1 1 2 0.1580
0 -2 1 0.1606
-1 -2 2 0.1404
-1 0 0 0.0593
1 0 0 0.1066
0 2 1 0.2363
0 -2 -1 0.2363
-2 0 -1 0.0813
2 0 1 0.1510
1 -2 1 0.1473
1 2 0 0.2168
1 1 0 0.1677
1 -2 -1 0.1964
2 -2 -1 0.1474
2 -1 -1 0.1155
-1 -2 0 0.1474
-1 2 1 0.1641
-2 2 1 0.1139
-2 1 1 0.0897
-1 -1 0 0.0965
2 0 -1 0.0935
1 -1 0 0.1245
-1 2 -2 0.1288
-1 0 -2 0.1098
-1 1 -1 0.1117
2 -1 0 0.0909
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Y1 C11 79.07(5) . . ?
O1 Y1 C13 129.00(5) . . ?
O1 Y1 C15 82.49(5) . . ?
O1 Y1 C14 111.60(5) . . ?
O1 Y1 C2 126.05(5) . . ?
O1 Y1 C12 106.43(5) . . ?
O1 Y1 C1 122.96(5) . . ?
O1 Y1 C3 96.80(5) . . ?
O1 Y1 C5 92.31(5) . . ?
O1 Y1 C21 96.81(6) . . ?
O1 Y1 C4 77.28(5) . . ?
C11 Y1 C15 30.50(5) . . ?
C11 Y1 C14 50.37(6) . . ?
C11 Y1 C2 154.27(6) . . ?
C11 Y1 C1 134.66(5) . . ?
C11 Y1 C3 174.63(6) . . ?
C13 Y1 C11 50.73(6) . . ?
C13 Y1 C15 50.49(5) . . ?
C13 Y1 C14 30.71(5) . . ?
C13 Y1 C2 103.55(6) . . ?
C13 Y1 C12 30.64(6) . . ?
C13 Y1 C1 92.95(6) . . ?
C13 Y1 C3 133.84(6) . . ?
C13 Y1 C4 142.77(6) . . ?
C14 Y1 C15 30.28(5) . . ?
C2 Y1 C15 135.89(6) . . ?
C2 Y1 C14 108.16(6) . . ?
C12 Y1 C11 30.75(6) . . ?
C12 Y1 C15 50.46(5) . . ?
C12 Y1 C14 50.47(5) . . ?
C12 Y1 C2 126.97(6) . . ?
C12 Y1 C1 123.31(6) . . ?
C12 Y1 C3 150.93(6) . . ?
C12 Y1 C4 173.03(6) . . ?
C1 Y1 C15 107.48(5) . . ?
C1 Y1 C14 84.38(5) . . ?
C1 Y1 C2 30.55(5) . . ?
C1 Y1 C3 50.56(5) . . ?
C3 Y1 C15 152.96(5) . . ?
C3 Y1 C14 134.91(6) . . ?
C3 Y1 C2 30.55(5) . . ?
C5 Y1 C11 132.17(5) . . ?
C5 Y1 C13 113.43(6) . . ?
C5 Y1 C15 102.05(5) . . ?
C5 Y1 C14 92.30(5) . . ?
C5 Y1 C2 50.88(5) . . ?
C5 Y1 C12 142.19(6) . . ?
C5 Y1 C1 30.90(5) . . ?
C5 Y1 C3 50.91(5) . . ?
C5 Y1 C4 30.87(5) . . ?
C21 Y1 C11 98.72(6) . . ?
C21 Y1 C13 98.81(6) . . ?
C21 Y1 C15 128.76(6) . . ?
C21 Y1 C14 128.99(6) . . ?
C21 Y1 C2 84.84(6) . . ?
C21 Y1 C12 81.81(6) . . ?
C21 Y1 C1 114.91(6) . . ?
C21 Y1 C3 78.25(6) . . ?
C21 Y1 C5 129.09(6) . . ?
C21 Y1 C4 103.79(6) . . ?
C4 Y1 C11 148.94(6) . . ?
C4 Y1 C15 125.45(5) . . ?
C4 Y1 C14 122.83(5) . . ?
C4 Y1 C2 50.56(5) . . ?
C4 Y1 C1 50.69(5) . . ?
C4 Y1 C3 30.62(5) . . ?
C27 O1 Y1 124.80(10) . . ?
C27 O1 C30 108.96(13) . . ?
C30 O1 Y1 126.23(10) . . ?
C15 C11 Y1 75.89(10) . . ?
C15 C11 C12 107.93(16) . . ?
C15 C11 C16 126.81(17) . . ?
C12 C11 Y1 74.34(10) . . ?
C12 C11 C16 125.07(17) . . ?
C16 C11 Y1 119.67(12) . . ?
C14 C13 Y1 75.90(10) . . ?
C14 C13 C18 126.36(19) . . ?
C12 C13 Y1 74.72(10) . . ?
C12 C13 C14 107.89(16) . . ?
C12 C13 C18 125.11(18) . . ?
C18 C13 Y1 122.68(12) . . ?
C11 C15 Y1 73.61(9) . . ?
C11 C15 C20 128.24(17) . . ?
C14 C15 Y1 74.66(9) . . ?
C14 C15 C11 108.04(15) . . ?
C14 C15 C20 122.61(17) . . ?
C20 C15 Y1 127.10(11) . . ?
C13 C14 Y1 73.40(10) . . ?
C13 C14 C19 127.27(18) . . ?
C15 C14 Y1 75.06(10) . . ?
C15 C14 C13 107.99(16) . . ?
C15 C14 C19 123.26(17) . . ?
C19 C14 Y1 128.36(12) . . ?
C1 C2 Y1 74.39(10) . . ?
C1 C2 C3 108.10(15) . . ?
C1 C2 C7 124.59(18) . . ?
C3 C2 Y1 74.62(10) . . ?
C3 C2 C7 126.57(18) . . ?
C7 C2 Y1 124.71(13) . . ?
C11 C12 Y1 74.91(10) . . ?
C11 C12 C17 124.49(19) . . ?
C13 C12 Y1 74.64(10) . . ?
C13 C12 C11 108.13(16) . . ?
C13 C12 C17 126.83(19) . . ?
C17 C12 Y1 123.20(12) . . ?
C2 C1 Y1 75.06(10) . . ?
C2 C1 C5 108.14(15) . . ?
C2 C1 C6 123.63(17) . . ?
C5 C1 Y1 73.71(10) . . ?
C5 C1 C6 127.16(17) . . ?
C6 C1 Y1 126.52(12) . . ?
C2 C3 Y1 74.83(10) . . ?
C2 C3 C4 108.01(15) . . ?
C2 C3 C8 126.89(18) . . ?
C4 C3 Y1 74.36(10) . . ?
C4 C3 C8 124.65(17) . . ?
C8 C3 Y1 122.83(12) . . ?
C1 C5 Y1 75.39(10) . . ?
C1 C5 C10 125.67(17) . . ?
C10 C5 Y1 119.62(12) . . ?
C4 C5 Y1 75.30(10) . . ?
C4 C5 C1 107.57(15) . . ?
C4 C5 C10 126.54(17) . . ?
C15 C20 H20A 109.5 . . ?
C15 C20 H20B 109.5 . . ?
C15 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O1 C27 H27A 110.7 . . ?
O1 C27 H27B 110.7 . . ?
O1 C27 C28 105.42(14) . . ?
H27A C27 H27B 108.8 . . ?
C28 C27 H27A 110.7 . . ?
C28 C27 H27B 110.7 . . ?
C26 C21 Y1 132.76(14) . . ?
C26 C21 C22 113.07(16) . . ?
C22 C21 Y1 113.39(13) . . ?
C21 C26 H26 118.1 . . ?
C25 C26 C21 123.86(18) . . ?
C25 C26 H26 118.1 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
C5 C10 H10A 109.5 . . ?
C5 C10 H10B 109.5 . . ?
C5 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C3 C4 Y1 75.02(10) . . ?
C3 C4 C5 108.16(15) . . ?
C3 C4 C9 124.21(17) . . ?
C5 C4 Y1 73.82(10) . . ?
C5 C4 C9 127.15(17) . . ?
C9 C4 Y1 123.38(12) . . ?
C27 C28 H28A 111.2 . . ?
C27 C28 H28B 111.2 . . ?
H28A C28 H28B 109.1 . . ?
C29 C28 C27 103.02(15) . . ?
C29 C28 H28A 111.2 . . ?
C29 C28 H28B 111.2 . . ?
C11 C16 H16A 109.5 . . ?
C11 C16 H16B 109.5 . . ?
C11 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C26 C25 H25 119.8 . . ?
C24 C25 C26 120.35(18) . . ?
C24 C25 H25 119.8 . . ?
C1 C6 H6A 109.5 . . ?
C1 C6 H6B 109.5 . . ?
C1 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 109.5 . . ?
C14 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C22 H22 117.9 . . ?
C23 C22 C21 124.28(18) . . ?
C23 C22 H22 117.9 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O1 C30 H30A 110.6 . . ?
O1 C30 H30B 110.6 . . ?
O1 C30 C29 105.92(15) . . ?
H30A C30 H30B 108.7 . . ?
C29 C30 H30A 110.6 . . ?
C29 C30 H30B 110.6 . . ?
C13 C18 H18A 109.5 . . ?
C13 C18 H18B 109.5 . . ?
C13 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C22 C23 H23 120.0 . . ?
C24 C23 C22 120.06(18) . . ?
C24 C23 H23 120.0 . . ?
C28 C29 H29A 111.3 . . ?
C28 C29 H29B 111.3 . . ?
C30 C29 C28 102.18(16) . . ?
C30 C29 H29A 111.3 . . ?
C30 C29 H29B 111.3 . . ?
H29A C29 H29B 109.2 . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
C3 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C25 C24 H24 120.8 . . ?
C23 C24 C25 118.32(18) . . ?
C23 C24 H24 120.8 . . ?
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
Y1 O1 2.3907(12) . ?
Y1 C11 2.6773(17) . ?
Y1 C13 2.6691(17) . ?
Y1 C15 2.7064(16) . ?
Y1 C14 2.7013(17) . ?
Y1 C2 2.6883(17) . ?
Y1 C12 2.6700(18) . ?
Y1 C1 2.6797(18) . ?
Y1 C3 2.6856(17) . ?
Y1 C5 2.6581(17) . ?
Y1 C21 2.4605(18) . ?
Y1 C4 2.6772(17) . ?
O1 C27 1.455(2) . ?
O1 C30 1.455(2) . ?
C11 C15 1.416(2) . ?
C11 C12 1.418(3) . ?
C11 C16 1.509(3) . ?
C13 C14 1.422(3) . ?
C13 C12 1.411(3) . ?
C13 C18 1.508(3) . ?
C15 C14 1.412(3) . ?
C15 C20 1.510(2) . ?
C14 C19 1.505(3) . ?
C2 C1 1.414(2) . ?
C2 C3 1.416(3) . ?
C2 C7 1.505(2) . ?
C12 C17 1.507(3) . ?
C1 C5 1.422(2) . ?
C1 C6 1.504(3) . ?
C3 C4 1.416(2) . ?
C3 C8 1.501(2) . ?
C5 C10 1.506(2) . ?
C5 C4 1.420(2) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.518(2) . ?
C21 C26 1.405(3) . ?
C21 C22 1.409(3) . ?
C26 H26 0.9500 . ?
C26 C25 1.392(3) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C9 C4 1.503(2) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.511(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C25 H25 0.9500 . ?
C25 C24 1.386(3) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C22 H22 0.9500 . ?
C22 C23 1.389(3) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C29 1.499(3) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C23 H23 0.9500 . ?
C23 C24 1.384(3) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C24 H24 0.9500 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Y1 O1 C27 C28 -172.45(12) . . . . ?
Y1 O1 C30 C29 -163.40(13) . . . . ?
Y1 C11 C15 C14 67.31(12) . . . . ?
Y1 C11 C15 C20 -124.67(17) . . . . ?
Y1 C11 C12 C13 -67.86(12) . . . . ?
Y1 C11 C12 C17 120.19(18) . . . . ?
Y1 C13 C14 C15 -67.69(12) . . . . ?
Y1 C13 C14 C19 125.93(18) . . . . ?
Y1 C13 C12 C11 68.04(12) . . . . ?
Y1 C13 C12 C17 -120.25(18) . . . . ?
Y1 C15 C14 C13 66.57(12) . . . . ?
Y1 C15 C14 C19 -126.38(17) . . . . ?
Y1 C2 C1 C5 66.87(12) . . . . ?
Y1 C2 C1 C6 -124.21(18) . . . . ?
Y1 C2 C3 C4 -67.55(12) . . . . ?
Y1 C2 C3 C8 119.92(19) . . . . ?
Y1 C1 C5 C10 -116.20(18) . . . . ?
Y1 C1 C5 C4 69.05(12) . . . . ?
Y1 C3 C4 C5 -66.96(12) . . . . ?
Y1 C3 C4 C9 120.45(18) . . . . ?
Y1 C5 C4 C3 67.76(12) . . . . ?
Y1 C5 C4 C9 -119.93(18) . . . . ?
Y1 C21 C26 C25 -168.60(15) . . . . ?
Y1 C21 C22 C23 168.80(17) . . . . ?
O1 C27 C28 C29 -29.0(2) . . . . ?
O1 C30 C29 C28 -33.1(2) . . . . ?
C11 C15 C14 Y1 -66.61(12) . . . . ?
C11 C15 C14 C13 -0.04(19) . . . . ?
C11 C15 C14 C19 167.01(16) . . . . ?
C15 C11 C12 Y1 69.09(12) . . . . ?
C15 C11 C12 C13 1.2(2) . . . . ?
C15 C11 C12 C17 -170.72(17) . . . . ?
C14 C13 C12 Y1 -69.29(12) . . . . ?
C14 C13 C12 C11 -1.3(2) . . . . ?
C14 C13 C12 C17 170.46(17) . . . . ?
C2 C1 C5 Y1 -67.77(13) . . . . ?
C2 C1 C5 C10 176.03(17) . . . . ?
C2 C1 C5 C4 1.3(2) . . . . ?
C2 C3 C4 Y1 67.86(12) . . . . ?
C2 C3 C4 C5 0.9(2) . . . . ?
C2 C3 C4 C9 -171.69(17) . . . . ?
C12 C11 C15 Y1 -68.04(12) . . . . ?
C12 C11 C15 C14 -0.73(19) . . . . ?
C12 C11 C15 C20 167.29(17) . . . . ?
C12 C13 C14 Y1 68.49(12) . . . . ?
C12 C13 C14 C15 0.80(19) . . . . ?
C12 C13 C14 C19 -165.58(17) . . . . ?
C1 C2 C3 Y1 67.44(12) . . . . ?
C1 C2 C3 C4 -0.1(2) . . . . ?
C1 C2 C3 C8 -172.63(18) . . . . ?
C1 C5 C4 Y1 -69.11(12) . . . . ?
C1 C5 C4 C3 -1.3(2) . . . . ?
C1 C5 C4 C9 170.97(17) . . . . ?
C3 C2 C1 Y1 -67.60(12) . . . . ?
C3 C2 C1 C5 -0.7(2) . . . . ?
C3 C2 C1 C6 168.19(17) . . . . ?
C20 C15 C14 Y1 124.55(16) . . . . ?
C20 C15 C14 C13 -168.88(15) . . . . ?
C20 C15 C14 C19 -1.8(3) . . . . ?
C27 O1 C30 C29 15.6(2) . . . . ?
C27 C28 C29 C30 37.7(2) . . . . ?
C21 C26 C25 C24 1.5(3) . . . . ?
C21 C22 C23 C24 2.6(3) . . . . ?
C26 C21 C22 C23 -2.4(3) . . . . ?
C26 C25 C24 C23 -1.4(3) . . . . ?
C10 C5 C4 Y1 116.21(18) . . . . ?
C10 C5 C4 C3 -176.03(17) . . . . ?
C10 C5 C4 C9 -3.7(3) . . . . ?
C16 C11 C15 Y1 116.70(18) . . . . ?
C16 C11 C15 C14 -175.99(17) . . . . ?
C16 C11 C15 C20 -8.0(3) . . . . ?
C16 C11 C12 Y1 -115.55(17) . . . . ?
C16 C11 C12 C13 176.59(17) . . . . ?
C16 C11 C12 C17 4.6(3) . . . . ?
C6 C1 C5 Y1 123.81(18) . . . . ?
C6 C1 C5 C10 7.6(3) . . . . ?
C6 C1 C5 C4 -167.14(18) . . . . ?
C22 C21 C26 C25 0.4(3) . . . . ?
C22 C23 C24 C25 -0.5(3) . . . . ?
C7 C2 C1 Y1 121.70(18) . . . . ?
C7 C2 C1 C5 -171.43(17) . . . . ?
C7 C2 C1 C6 -2.5(3) . . . . ?
C7 C2 C3 Y1 -122.09(19) . . . . ?
C7 C2 C3 C4 170.36(18) . . . . ?
C7 C2 C3 C8 -2.2(3) . . . . ?
C30 O1 C27 C28 8.6(2) . . . . ?
C18 C13 C14 Y1 -120.42(18) . . . . ?
C18 C13 C14 C15 171.89(17) . . . . ?
C18 C13 C14 C19 5.5(3) . . . . ?
C18 C13 C12 Y1 119.48(18) . . . . ?
C18 C13 C12 C11 -172.49(17) . . . . ?
C18 C13 C12 C17 -0.8(3) . . . . ?
C8 C3 C4 Y1 -119.40(18) . . . . ?
C8 C3 C4 C5 173.64(17) . . . . ?
C8 C3 C4 C9 1.0(3) . . . . ?
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
0.0001 1.0025 0.9983 0.0230 -0.0272 -0.0481
0.9992 -0.0024 -1.9992 -0.0853 -0.0372 0.0426
0.9994 0.9985 -1.9996 -0.1000 -0.0463 0.0051
-0.9987 2.0040 1.9984 0.0558 0.0189 -0.1177
-0.9989 1.0032 1.9988 0.0706 0.0281 -0.0801
-0.0007 -2.0000 0.9996 0.0672 0.0002 0.0646
-0.9997 -1.9993 2.0001 0.1148 0.0555 0.0325
-0.9989 -0.0010 0.0018 0.0098 0.0733 -0.0216
0.9989 0.0010 -0.0018 -0.0098 -0.0733 0.0216
0.0004 2.0034 0.9979 0.0083 -0.0363 -0.0856
-0.0004 -2.0034 -0.9979 -0.0083 0.0363 0.0856
-1.9976 -0.0036 -0.9952 -0.0182 0.1647 -0.0327
1.9976 0.0036 0.9952 0.0182 -0.1647 0.0327
0.9982 -1.9991 0.9978 0.0574 -0.0731 0.0862
0.9994 2.0027 -0.0026 -0.0392 -0.0916 -0.0535
0.9991 1.0018 -0.0022 -0.0245 -0.0824 -0.0160
0.9985 -2.0024 -0.9996 -0.0181 -0.0370 0.1072
1.9974 -2.0014 -1.0014 -0.0279 -0.1103 0.1288
1.9976 -1.0006 -1.0018 -0.0426 -0.1194 0.0912
-0.9994 -2.0027 0.0026 0.0392 0.0916 0.0535
-0.9985 2.0024 0.9996 0.0181 0.0370 -0.1072
-1.9974 2.0014 1.0014 0.0279 0.1103 -0.1288
-1.9976 1.0006 1.0018 0.0426 0.1194 -0.0912
-0.9991 -1.0018 0.0022 0.0245 0.0824 0.0160
1.9979 0.0003 -1.0022 -0.0573 -0.1286 0.0537
0.9986 -0.9999 -0.0013 0.0049 -0.0642 0.0591
-0.9981 1.9974 -1.9965 -0.0952 0.0912 -0.0757
-0.9986 -0.0043 -1.9957 -0.0657 0.1094 -0.0006
-0.9985 0.9982 -0.9974 -0.0427 0.0822 -0.0486
1.9975 -0.9989 -0.0031 -0.0048 -0.1375 0.0807
