#------------------------------------------------------------------------------
#$Date: 2024-07-05 19:40:57 +0300 (Fri, 05 Jul 2024) $
#$Revision: 293106 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/52/7715245.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_7715245
loop_
_publ_author_name
'Franke, Maurice'
'Klingsiek, Maximilian J.'
'Buth, Julian'
'Lamm, Jan-Hendrik'
'Neumann, Beate'
'Stammler, Hans-Georg'
'Mitzel, Norbert W.'
_publ_section_title
;
 Hexadentate poly-Lewis acids based on the bowl-shaped
 tribenzotriquinacene.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7751
_journal_page_last               7762
_journal_paper_doi               10.1039/d4dt00379a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C31 H34'
_chemical_formula_sum            'C31 H34'
_chemical_formula_weight         406.58
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-20
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2024-01-16 deposited with the CCDC.	2024-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                99.294(3)
_cell_angle_beta                 104.180(3)
_cell_angle_gamma                93.662(3)
_cell_formula_units_Z            2
_cell_length_a                   9.0140(4)
_cell_length_b                   9.3643(3)
_cell_length_c                   14.7850(5)
_cell_measurement_reflns_used    5009
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.3050
_cell_measurement_theta_min      4.8300
_cell_volume                     1187.09(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -57.00 -10.00   1.00    5.50    --  -38.50 125.00-180.00   47
  2  ω    -56.00  32.00   1.00    5.50    --  -38.50  37.00  90.00   88
  3  ω   -114.00 -13.00   1.00    5.50    --  -38.50 -19.00 -90.00  101
  4  ω    -82.00 -17.00   1.00    5.50    --  -38.50 125.00 120.00   65
  5  ω     47.00  93.00   1.00    5.50    --   42.70-125.00  30.00   46
  6  ω     85.00 113.00   1.00   31.50    --  111.00-125.00   0.00   28
  7  ω    100.00 177.00   1.00   31.50    --  111.00  15.00  30.00   77
  8  ω     46.00  79.00   1.00   31.50    --  111.00 -61.00 120.00   33
  9  ω     41.00 113.00   1.00   31.50    --  111.00-125.00-120.00   72
 10  ω     55.00 137.00   1.00   31.50    --  111.00 -61.00-150.00   82
 11  ω    139.00 178.00   1.00   31.50    --  111.00  77.00-180.00   39
 12  ω     39.00 106.00   1.00   31.50    --  111.00 -94.00 120.00   67
 13  ω     85.00 178.00   1.00   31.50    --  111.00  61.00 -90.00   93
 14  ω    149.00 177.00   1.00   31.50    --  111.00  77.00 -60.00   28
 15  ω     31.00 107.00   1.00   31.50    --  111.00 -94.00   0.00   76
 16  ω     97.00 163.00   1.00   31.50    --  111.00 125.00-150.00   66
 17  ω     98.00 134.00   1.00   31.50    --  111.00 125.00   0.00   36
 18  ω     33.00  63.00   1.00   31.50    --  111.00 -94.00-120.00   30
 19  ω     74.00  99.00   1.00   31.50    --  111.00 -94.00-120.00   25
 20  ω    112.00 137.00   1.00   31.50    --  111.00 -61.00 120.00   25
 21  ω     95.00 169.00   1.00   31.50    --  111.00  30.00 -30.00   74
 22  ω     62.00 107.00   1.00   31.50    --  111.00 -94.00  60.00   45
 23  ω     38.00  76.00   1.00   31.50    --  111.00 -94.00  30.00   38
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1721229000
_diffrn_orient_matrix_UB_12      -0.0369919000
_diffrn_orient_matrix_UB_13      -0.0075814000
_diffrn_orient_matrix_UB_21      0.0207695000
_diffrn_orient_matrix_UB_22      0.0912957000
_diffrn_orient_matrix_UB_23      0.0996269000
_diffrn_orient_matrix_UB_31      -0.0372057000
_diffrn_orient_matrix_UB_32      0.1357013000
_diffrn_orient_matrix_UB_33      -0.0443608000
_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  0.0228
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9704
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.342
_diffrn_reflns_theta_min         3.136
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.473
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.930
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.104a (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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_description       plate
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         4856
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0419
_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)+(0.0550P)²+0.3012P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1109
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4125
_reflns_number_total             4856
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt00379a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7715245--7715251.cif.'
_cod_database_code               7715245
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C31 H34'
_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   0.991
_shelx_estimated_absorpt_t_min   0.945
_reflns_odcompleteness_completeness 99.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
;
_olex2_date_sample_data_collection 2021-07-19
_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 1.104
_oxdiff_exptl_absorpt_empirical_full_min 0.908
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
C1 C 0.50738(14) 0.73799(12) 0.27359(8) 0.0172(2) Uani 1 1 d . . . . .
H1 H 0.556(2) 0.8001(18) 0.3370(12) 0.022(4) Uiso 1 1 d . . . . .
C2 C 0.32953(14) 0.70778(12) 0.25873(8) 0.0177(2) Uani 1 1 d . . . . .
C3 C 0.26116(14) 0.77221(12) 0.17146(8) 0.0178(2) Uani 1 1 d . . . . .
C4 C 0.10606(14) 0.77569(13) 0.12753(9) 0.0204(2) Uani 1 1 d . . . . .
H4 H 0.0248(19) 0.7370(17) 0.1528(12) 0.020(4) Uiso 1 1 d . . . . .
C5 C 0.06664(15) 0.83633(13) 0.04591(9) 0.0218(3) Uani 1 1 d . . . . .
H5 H -0.041(2) 0.8365(18) 0.0151(12) 0.024(4) Uiso 1 1 d . . . . .
C6 C 0.18058(15) 0.89309(13) 0.00877(9) 0.0220(3) Uani 1 1 d . . . . .
H6 H 0.152(2) 0.9337(19) -0.0492(13) 0.027(4) Uiso 1 1 d . . . . .
C7 C 0.33498(15) 0.89041(13) 0.05309(9) 0.0206(2) Uani 1 1 d . . . . .
H7 H 0.413(2) 0.9290(17) 0.0264(12) 0.020(4) Uiso 1 1 d . . . . .
C8 C 0.37475(14) 0.82964(12) 0.13461(9) 0.0178(2) Uani 1 1 d . . . . .
C9 C 0.53571(13) 0.81537(12) 0.19199(8) 0.0168(2) Uani 1 1 d . . . . .
C10 C 0.61568(13) 0.70772(12) 0.13736(8) 0.0168(2) Uani 1 1 d . . . . .
C11 C 0.66039(14) 0.72007(13) 0.05506(9) 0.0200(2) Uani 1 1 d . . . . .
H11 H 0.643(2) 0.809(2) 0.0262(13) 0.029(4) Uiso 1 1 d . . . . .
C12 C 0.72905(14) 0.60753(14) 0.01339(9) 0.0215(3) Uani 1 1 d . . . . .
H12 H 0.759(2) 0.6140(18) -0.0429(13) 0.026(4) Uiso 1 1 d . . . . .
C13 C 0.75545(15) 0.48482(13) 0.05457(9) 0.0223(3) Uani 1 1 d . . . . .
H13 H 0.804(2) 0.4072(19) 0.0245(13) 0.027(4) Uiso 1 1 d . . . . .
C14 C 0.71024(14) 0.47215(13) 0.13661(9) 0.0209(2) Uani 1 1 d . . . . .
H14 H 0.726(2) 0.3871(19) 0.1647(12) 0.024(4) Uiso 1 1 d . . . . .
C15 C 0.63928(13) 0.58391(13) 0.17745(8) 0.0177(2) Uani 1 1 d . . . . .
C16 C 0.57619(14) 0.58816(12) 0.26409(8) 0.0177(2) Uani 1 1 d . . . . .
C17 C 0.43610(14) 0.47708(13) 0.24409(8) 0.0185(2) Uani 1 1 d . . . . .
C18 C 0.43287(16) 0.32596(13) 0.22981(9) 0.0229(3) Uani 1 1 d . . . . .
H18 H 0.528(2) 0.281(2) 0.2327(13) 0.029(4) Uiso 1 1 d . . . . .
C19 C 0.29232(17) 0.24077(13) 0.20868(9) 0.0247(3) Uani 1 1 d . . . . .
H19 H 0.288(2) 0.136(2) 0.1977(13) 0.027(4) Uiso 1 1 d . . . . .
C20 C 0.15651(16) 0.30610(14) 0.20200(9) 0.0240(3) Uani 1 1 d . . . . .
H20 H 0.061(2) 0.2484(19) 0.1878(13) 0.028(4) Uiso 1 1 d . . . . .
C21 C 0.15943(15) 0.45719(14) 0.21720(9) 0.0214(3) Uani 1 1 d . . . . .
H21 H 0.066(2) 0.5015(18) 0.2138(12) 0.025(4) Uiso 1 1 d . . . . .
C22 C 0.30071(14) 0.54219(12) 0.23862(8) 0.0178(2) Uani 1 1 d . . . . .
C23 C 0.27128(15) 0.77004(13) 0.34516(9) 0.0219(3) Uani 1 1 d . . . . .
H23A H 0.327(2) 0.7290(18) 0.4020(12) 0.022(4) Uiso 1 1 d . . . . .
H23B H 0.158(2) 0.7342(19) 0.3335(13) 0.027(4) Uiso 1 1 d . . . . .
C24 C 0.28816(18) 0.93548(15) 0.37153(10) 0.0280(3) Uani 1 1 d . . . . .
H24A H 0.399(2) 0.976(2) 0.3800(14) 0.037(5) Uiso 1 1 d . . . . .
H24B H 0.225(2) 0.979(2) 0.3199(15) 0.038(5) Uiso 1 1 d . . . . .
C25 C 0.2420(2) 0.98616(18) 0.46343(11) 0.0373(3) Uani 1 1 d . . . . .
H25A H 0.132(2) 0.945(2) 0.4583(14) 0.038(5) Uiso 1 1 d . . . . .
H25B H 0.311(3) 0.949(2) 0.5185(17) 0.049(6) Uiso 1 1 d . . . . .
H25C H 0.251(2) 1.098(2) 0.4807(15) 0.044(5) Uiso 1 1 d . . . . .
C26 C 0.62856(14) 0.96704(13) 0.22702(9) 0.0210(2) Uani 1 1 d . . . . .
H26A H 0.572(2) 1.0258(19) 0.2671(12) 0.024(4) Uiso 1 1 d . . . . .
H26B H 0.627(2) 1.0163(18) 0.1696(12) 0.023(4) Uiso 1 1 d . . . . .
C27 C 0.79561(16) 0.97005(14) 0.28180(10) 0.0259(3) Uani 1 1 d . . . . .
H27A H 0.852(2) 0.920(2) 0.2391(14) 0.036(5) Uiso 1 1 d . . . . .
H27B H 0.802(2) 0.918(2) 0.3379(14) 0.031(4) Uiso 1 1 d . . . . .
C28 C 0.87130(18) 1.12619(16) 0.31895(12) 0.0333(3) Uani 1 1 d . . . . .
H28A H 0.818(2) 1.178(2) 0.3646(15) 0.042(5) Uiso 1 1 d . . . . .
H28B H 0.859(2) 1.180(2) 0.2638(15) 0.039(5) Uiso 1 1 d . . . . .
H28C H 0.980(3) 1.127(2) 0.3509(17) 0.052(6) Uiso 1 1 d . . . . .
C29 C 0.70337(15) 0.57100(14) 0.35147(9) 0.0219(3) Uani 1 1 d . . . . .
H29A H 0.789(2) 0.6506(19) 0.3634(12) 0.025(4) Uiso 1 1 d . . . . .
H29B H 0.749(2) 0.478(2) 0.3359(13) 0.031(4) Uiso 1 1 d . . . . .
C30 C 0.65159(17) 0.56716(16) 0.44159(10) 0.0287(3) Uani 1 1 d . . . . .
H30A H 0.602(2) 0.659(2) 0.4576(13) 0.032(4) Uiso 1 1 d . . . . .
H30B H 0.572(2) 0.481(2) 0.4311(14) 0.036(5) Uiso 1 1 d . . . . .
C31 C 0.7851(2) 0.5574(2) 0.52549(11) 0.0408(4) Uani 1 1 d . . . . .
H31A H 0.840(3) 0.460(3) 0.5128(17) 0.056(6) Uiso 1 1 d . . . . .
H31B H 0.864(3) 0.638(2) 0.5330(16) 0.048(6) Uiso 1 1 d . . . . .
H31C H 0.744(3) 0.557(3) 0.5858(18) 0.055(6) Uiso 1 1 d . . . . .
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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0110
2 0 -1 0.0594
-2 0 1 0.0594
0 1 -1 0.0295
0 -1 1 0.0295
0 0 -1 0.0110
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
C2 C1 H1 110.5(10) . . ?
C2 C1 C9 108.06(9) . . ?
C2 C1 C16 108.45(9) . . ?
C9 C1 H1 110.7(9) . . ?
C9 C1 C16 107.99(9) . . ?
C16 C1 H1 111.0(9) . . ?
C3 C2 C1 103.94(9) . . ?
C3 C2 C22 111.86(10) . . ?
C3 C2 C23 112.72(10) . . ?
C22 C2 C1 103.53(9) . . ?
C22 C2 C23 109.88(9) . . ?
C23 C2 C1 114.47(10) . . ?
C4 C3 C2 127.90(11) . . ?
C8 C3 C2 111.76(10) . . ?
C8 C3 C4 120.32(11) . . ?
C3 C4 H4 121.5(10) . . ?
C5 C4 C3 119.14(11) . . ?
C5 C4 H4 119.3(10) . . ?
C4 C5 H5 118.6(10) . . ?
C6 C5 C4 120.47(11) . . ?
C6 C5 H5 120.9(10) . . ?
C5 C6 H6 120.0(11) . . ?
C7 C6 C5 120.24(11) . . ?
C7 C6 H6 119.8(11) . . ?
C6 C7 H7 119.7(10) . . ?
C6 C7 C8 119.43(11) . . ?
C8 C7 H7 120.9(10) . . ?
C3 C8 C7 120.40(11) . . ?
C3 C8 C9 112.47(10) . . ?
C7 C8 C9 127.13(11) . . ?
C8 C9 C1 103.74(9) . . ?
C8 C9 C10 111.75(10) . . ?
C8 C9 C26 109.92(9) . . ?
C10 C9 C1 103.94(9) . . ?
C10 C9 C26 112.97(10) . . ?
C26 C9 C1 114.08(10) . . ?
C11 C10 C9 127.61(10) . . ?
C15 C10 C9 112.08(10) . . ?
C15 C10 C11 120.28(11) . . ?
C10 C11 H11 120.4(11) . . ?
C12 C11 C10 119.38(11) . . ?
C12 C11 H11 120.3(11) . . ?
C11 C12 H12 120.2(10) . . ?
C11 C12 C13 120.33(11) . . ?
C13 C12 H12 119.4(10) . . ?
C12 C13 H13 119.2(10) . . ?
C14 C13 C12 120.30(11) . . ?
C14 C13 H13 120.5(10) . . ?
C13 C14 H14 121.0(10) . . ?
C13 C14 C15 119.31(11) . . ?
C15 C14 H14 119.7(10) . . ?
C10 C15 C14 120.37(11) . . ?
C10 C15 C16 112.29(10) . . ?
C14 C15 C16 127.32(11) . . ?
C15 C16 C1 103.68(9) . . ?
C15 C16 C17 111.19(10) . . ?
C15 C16 C29 110.84(10) . . ?
C17 C16 C1 103.48(9) . . ?
C17 C16 C29 112.78(9) . . ?
C29 C16 C1 114.33(10) . . ?
C18 C17 C16 127.28(11) . . ?
C22 C17 C16 112.28(10) . . ?
C22 C17 C18 120.42(12) . . ?
C17 C18 H18 120.2(11) . . ?
C19 C18 C17 119.31(12) . . ?
C19 C18 H18 120.5(11) . . ?
C18 C19 H19 120.1(11) . . ?
C18 C19 C20 120.21(12) . . ?
C20 C19 H19 119.7(11) . . ?
C19 C20 H20 120.3(11) . . ?
C19 C20 C21 120.65(12) . . ?
C21 C20 H20 119.0(11) . . ?
C20 C21 H21 120.4(10) . . ?
C20 C21 C22 118.94(12) . . ?
C22 C21 H21 120.7(10) . . ?
C17 C22 C2 112.20(10) . . ?
C17 C22 C21 120.47(11) . . ?
C21 C22 C2 127.33(11) . . ?
C2 C23 H23A 108.8(10) . . ?
C2 C23 H23B 109.7(10) . . ?
H23A C23 H23B 105.6(13) . . ?
C24 C23 C2 115.58(10) . . ?
C24 C23 H23A 109.0(10) . . ?
C24 C23 H23B 107.7(10) . . ?
C23 C24 H24A 110.2(11) . . ?
C23 C24 H24B 111.0(12) . . ?
C23 C24 C25 111.59(12) . . ?
H24A C24 H24B 106.0(15) . . ?
C25 C24 H24A 108.7(12) . . ?
C25 C24 H24B 109.2(12) . . ?
C24 C25 H25A 111.1(12) . . ?
C24 C25 H25B 110.2(13) . . ?
C24 C25 H25C 111.9(12) . . ?
H25A C25 H25B 106.7(16) . . ?
H25A C25 H25C 108.6(16) . . ?
H25B C25 H25C 108.1(18) . . ?
C9 C26 H26A 106.5(10) . . ?
C9 C26 H26B 108.9(10) . . ?
H26A C26 H26B 107.1(13) . . ?
C27 C26 C9 116.19(10) . . ?
C27 C26 H26A 110.0(10) . . ?
C27 C26 H26B 107.8(10) . . ?
C26 C27 H27A 108.6(12) . . ?
C26 C27 H27B 110.2(11) . . ?
C26 C27 C28 111.18(11) . . ?
H27A C27 H27B 109.2(15) . . ?
C28 C27 H27A 109.0(11) . . ?
C28 C27 H27B 108.6(11) . . ?
C27 C28 H28A 109.9(12) . . ?
C27 C28 H28B 109.0(12) . . ?
C27 C28 H28C 110.7(14) . . ?
H28A C28 H28B 107.3(16) . . ?
H28A C28 H28C 109.2(18) . . ?
H28B C28 H28C 110.6(17) . . ?
C16 C29 H29A 109.0(10) . . ?
C16 C29 H29B 108.7(11) . . ?
H29A C29 H29B 105.5(14) . . ?
C30 C29 C16 115.41(11) . . ?
C30 C29 H29A 110.0(10) . . ?
C30 C29 H29B 107.8(10) . . ?
C29 C30 H30A 109.1(10) . . ?
C29 C30 H30B 109.8(11) . . ?
C29 C30 C31 112.09(13) . . ?
H30A C30 H30B 108.1(16) . . ?
C31 C30 H30A 108.6(11) . . ?
C31 C30 H30B 109.1(11) . . ?
C30 C31 H31A 111.5(13) . . ?
C30 C31 H31B 108.5(13) . . ?
C30 C31 H31C 109.3(14) . . ?
H31A C31 H31B 105.9(18) . . ?
H31A C31 H31C 108.5(17) . . ?
H31B C31 H31C 113.1(19) . . ?
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
C1 H1 0.999(18) . ?
C1 C2 1.5645(16) . ?
C1 C9 1.5671(15) . ?
C1 C16 1.5695(15) . ?
C2 C3 1.5226(16) . ?
C2 C22 1.5239(16) . ?
C2 C23 1.5413(16) . ?
C3 C4 1.3947(17) . ?
C3 C8 1.3899(17) . ?
C4 H4 0.975(17) . ?
C4 C5 1.3936(18) . ?
C5 H5 0.970(18) . ?
C5 C6 1.3928(19) . ?
C6 H6 0.977(18) . ?
C6 C7 1.3892(18) . ?
C7 H7 0.966(17) . ?
C7 C8 1.3932(17) . ?
C8 C9 1.5169(16) . ?
C9 C10 1.5177(16) . ?
C9 C26 1.5441(16) . ?
C10 C11 1.3916(17) . ?
C10 C15 1.3901(16) . ?
C11 H11 0.998(18) . ?
C11 C12 1.3905(18) . ?
C12 H12 0.944(18) . ?
C12 C13 1.3921(18) . ?
C13 H13 0.973(18) . ?
C13 C14 1.3907(18) . ?
C14 H14 0.959(17) . ?
C14 C15 1.3927(17) . ?
C15 C16 1.5196(16) . ?
C16 C17 1.5212(17) . ?
C16 C29 1.5408(16) . ?
C17 C18 1.3941(17) . ?
C17 C22 1.3893(17) . ?
C18 H18 0.973(19) . ?
C18 C19 1.3913(19) . ?
C19 H19 0.967(18) . ?
C19 C20 1.392(2) . ?
C20 H20 0.946(19) . ?
C20 C21 1.3937(18) . ?
C21 H21 0.953(18) . ?
C21 C22 1.3953(18) . ?
C23 H23A 1.015(17) . ?
C23 H23B 1.016(19) . ?
C23 C24 1.5235(18) . ?
C24 H24A 1.02(2) . ?
C24 H24B 0.99(2) . ?
C24 C25 1.5294(19) . ?
C25 H25A 1.02(2) . ?
C25 H25B 1.02(2) . ?
C25 H25C 1.03(2) . ?
C26 H26A 0.998(18) . ?
C26 H26B 1.027(17) . ?
C26 C27 1.5211(18) . ?
C27 H27A 0.98(2) . ?
C27 H27B 1.017(18) . ?
C27 C28 1.5279(18) . ?
C28 H28A 1.00(2) . ?
C28 H28B 1.02(2) . ?
C28 H28C 0.97(3) . ?
C29 H29A 1.000(18) . ?
C29 H29B 1.006(19) . ?
C29 C30 1.5207(18) . ?
C30 H30A 1.012(19) . ?
C30 H30B 1.01(2) . ?
C30 C31 1.521(2) . ?
C31 H31A 1.08(2) . ?
C31 H31B 0.98(2) . ?
C31 H31C 1.04(2) . ?
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
C1 C2 C3 C4 -179.63(11) . . . . ?
C1 C2 C3 C8 1.68(13) . . . . ?
C1 C2 C22 C17 2.52(13) . . . . ?
C1 C2 C22 C21 -177.81(11) . . . . ?
C1 C2 C23 C24 65.90(14) . . . . ?
C1 C9 C10 C11 176.87(12) . . . . ?
C1 C9 C10 C15 -1.40(13) . . . . ?
C1 C9 C26 C27 66.89(14) . . . . ?
C1 C16 C17 C18 -179.82(12) . . . . ?
C1 C16 C17 C22 1.59(13) . . . . ?
C1 C16 C29 C30 65.77(14) . . . . ?
C2 C1 C9 C8 1.08(12) . . . . ?
C2 C1 C9 C10 -115.90(10) . . . . ?
C2 C1 C9 C26 120.65(10) . . . . ?
C2 C1 C16 C15 116.19(10) . . . . ?
C2 C1 C16 C17 0.03(12) . . . . ?
C2 C1 C16 C29 -123.02(11) . . . . ?
C2 C3 C4 C5 -178.07(11) . . . . ?
C2 C3 C8 C7 178.38(10) . . . . ?
C2 C3 C8 C9 -1.07(14) . . . . ?
C2 C23 C24 C25 -174.44(12) . . . . ?
C3 C2 C22 C17 113.84(11) . . . . ?
C3 C2 C22 C21 -66.49(15) . . . . ?
C3 C2 C23 C24 -52.62(15) . . . . ?
C3 C4 C5 C6 -0.16(18) . . . . ?
C3 C8 C9 C1 -0.04(13) . . . . ?
C3 C8 C9 C10 111.33(11) . . . . ?
C3 C8 C9 C26 -122.41(11) . . . . ?
C4 C3 C8 C7 -0.42(18) . . . . ?
C4 C3 C8 C9 -179.87(10) . . . . ?
C4 C5 C6 C7 -0.31(19) . . . . ?
C5 C6 C7 C8 0.41(18) . . . . ?
C6 C7 C8 C3 -0.05(18) . . . . ?
C6 C7 C8 C9 179.32(11) . . . . ?
C7 C8 C9 C1 -179.45(11) . . . . ?
C7 C8 C9 C10 -68.07(15) . . . . ?
C7 C8 C9 C26 58.19(15) . . . . ?
C8 C3 C4 C5 0.52(18) . . . . ?
C8 C9 C10 C11 65.63(15) . . . . ?
C8 C9 C10 C15 -112.65(11) . . . . ?
C8 C9 C26 C27 -177.10(11) . . . . ?
C9 C1 C2 C3 -1.64(12) . . . . ?
C9 C1 C2 C22 115.38(10) . . . . ?
C9 C1 C2 C23 -125.02(10) . . . . ?
C9 C1 C16 C15 -0.67(12) . . . . ?
C9 C1 C16 C17 -116.83(10) . . . . ?
C9 C1 C16 C29 120.12(11) . . . . ?
C9 C10 C11 C12 -178.23(11) . . . . ?
C9 C10 C15 C14 179.51(11) . . . . ?
C9 C10 C15 C16 1.05(14) . . . . ?
C9 C26 C27 C28 -175.68(11) . . . . ?
C10 C9 C26 C27 -51.53(14) . . . . ?
C10 C11 C12 C13 -1.19(18) . . . . ?
C10 C15 C16 C1 -0.20(13) . . . . ?
C10 C15 C16 C17 110.39(11) . . . . ?
C10 C15 C16 C29 -123.33(11) . . . . ?
C11 C10 C15 C14 1.10(18) . . . . ?
C11 C10 C15 C16 -177.37(11) . . . . ?
C11 C12 C13 C14 1.45(19) . . . . ?
C12 C13 C14 C15 -0.43(19) . . . . ?
C13 C14 C15 C10 -0.84(19) . . . . ?
C13 C14 C15 C16 177.38(12) . . . . ?
C14 C15 C16 C1 -178.54(12) . . . . ?
C14 C15 C16 C17 -67.95(16) . . . . ?
C14 C15 C16 C29 58.34(16) . . . . ?
C15 C10 C11 C12 -0.08(18) . . . . ?
C15 C16 C17 C18 69.46(15) . . . . ?
C15 C16 C17 C22 -109.13(11) . . . . ?
C15 C16 C29 C30 -177.49(10) . . . . ?
C16 C1 C2 C3 -118.46(10) . . . . ?
C16 C1 C2 C22 -1.43(12) . . . . ?
C16 C1 C2 C23 118.16(10) . . . . ?
C16 C1 C9 C8 118.19(10) . . . . ?
C16 C1 C9 C10 1.22(12) . . . . ?
C16 C1 C9 C26 -122.24(10) . . . . ?
C16 C17 C18 C19 -177.58(11) . . . . ?
C16 C17 C22 C2 -2.69(14) . . . . ?
C16 C17 C22 C21 177.61(10) . . . . ?
C16 C29 C30 C31 -177.22(12) . . . . ?
C17 C16 C29 C30 -52.09(14) . . . . ?
C17 C18 C19 C20 -0.06(19) . . . . ?
C18 C17 C22 C2 178.61(11) . . . . ?
C18 C17 C22 C21 -1.08(18) . . . . ?
C18 C19 C20 C21 -0.61(19) . . . . ?
C19 C20 C21 C22 0.43(18) . . . . ?
C20 C21 C22 C2 -179.24(11) . . . . ?
C20 C21 C22 C17 0.41(18) . . . . ?
C22 C2 C3 C4 69.31(15) . . . . ?
C22 C2 C3 C8 -109.38(11) . . . . ?
C22 C2 C23 C24 -178.12(11) . . . . ?
C22 C17 C18 C19 0.90(18) . . . . ?
C23 C2 C3 C4 -55.11(16) . . . . ?
C23 C2 C3 C8 126.20(11) . . . . ?
C23 C2 C22 C17 -120.17(11) . . . . ?
C23 C2 C22 C21 59.49(16) . . . . ?
C26 C9 C10 C11 -58.95(16) . . . . ?
C26 C9 C10 C15 122.78(11) . . . . ?
C29 C16 C17 C18 -55.75(16) . . . . ?
C29 C16 C17 C22 125.67(11) . . . . ?
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
0.0022 0.0006 1.0009 -0.0080 0.0998 -0.0444
2.0020 -0.0029 -1.0087 -0.3368 -0.0592 -0.0301
-2.0020 0.0029 1.0087 0.3368 0.0592 0.0301
0.0004 1.0010 -1.0016 -0.0295 -0.0084 0.1803
-0.0004 -1.0010 1.0016 0.0295 0.0084 -0.1803
-0.0022 -0.0006 -1.0009 0.0080 -0.0998 0.0444
