#------------------------------------------------------------------------------
#$Date: 2020-12-04 04:18:22 +0200 (Fri, 04 Dec 2020) $
#$Revision: 259514 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/53/4135348.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_4135348
loop_
_publ_author_name
'Wu, Yitao'
'Zhou, Jiong'
'Li, Errui'
'Wang, Mengbin'
'Jie, Kecheng'
'Zhu, Huangtianzhi'
'Huang, Feihe'
_publ_section_title
;
 Selective Separation of Methylfuran and Dimethylfuran by Nonporous
 Adaptive Crystals of Pillararenes.
;
_journal_issue                   46
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19722
_journal_page_last               19730
_journal_paper_doi               10.1021/jacs.0c09757
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'C55 H60 Br10 O10, C5 H6 O'
_chemical_formula_sum            'C60 H66 Br10 O11'
_chemical_formula_weight         1762.22
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.4691(9)
_cell_length_b                   20.7774(8)
_cell_length_c                   12.8545(5)
_cell_measurement_reflns_used    9354
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      52.499
_cell_measurement_theta_min      3.703
_cell_volume                     6535.3(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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_temperature      169.98
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.1197
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            62688
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.057
_diffrn_reflns_theta_min         3.143
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.359
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.4461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1694 before and 0.1023 after correction. The Ratio of minimum to maximum transmission is 0.5942. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_description       block
_exptl_crystal_F_000             3456
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.334
_refine_diff_density_min         -1.762
_refine_diff_density_rms         0.270
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         6244
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.1304
_refine_ls_R_factor_gt           0.0982
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2904
_refine_ls_wR_factor_ref         0.3197
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4238
_reflns_number_total             6244
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja0c09757_si_006.cif
_cod_data_source_block           191024wyt_p5
_cod_depositor_comments
'Adding full bibliography for 4135342--4135349.cif.'
_cod_database_code               4135348
_shelx_shelxl_version_number     2016/6
_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   0.739
_shelx_estimated_absorpt_t_min   0.674
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C33-O6
 1.4 with sigma of 0.02
 C30-C31
 1.48 with sigma of 0.02
 C30-C29
 1.5 with sigma of 0.02
 C30-O6 = C33-O6
 1.48 with sigma of 0.02
 C32-C31
 1.4 with sigma of 0.02
 C30-C31 = C33-C32
 1.4 with sigma of 0.02
 O6-C32
 2.4 with sigma of 0.02
 O6-C29 \\sim C29-C31
 with sigma of 0.02
3. Restrained planarity
 O6, C29, C30, C31, C33
 with sigma of 0.1
 O6, C29, C30, C31, C32, C33
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O6 \\sim C29 \\sim C30 \\sim C31 \\sim C33: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
O6 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(C29) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Fixed Sof: H18A(0.5) H18B(0.5) O6(0.5) C29(0.5) H29B(0.5) H29A(0.5) H29C(0.5)
 C30(0.5) C31(0.5) H31(0.5) C32(0.5) H32(0.5) C33(0.5) H33(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C11(H11A,H11B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B),
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
  C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C10(H10), C13(H13), C16(H16), C31(H31), C32(H32), C33(H33)
6.c Idealised Me refined as rotating group:
 C29(H29B,H29A,H29C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, 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
Br1 Br 0.28266(5) 0.94821(6) 0.09551(9) 0.0571(4) Uani 1 1 d . . . . .
Br2 Br 0.34287(6) 0.91182(7) 0.79581(12) 0.0785(5) Uani 1 1 d . . . . .
Br3 Br 0.34259(5) 0.69609(6) 0.65422(11) 0.0625(4) Uani 1 1 d . . . . .
Br4 Br 0.75390(5) 0.64643(6) 0.49799(11) 0.0659(5) Uani 1 1 d . . . . .
Br5 Br 0.69060(5) 0.49769(5) 0.12930(8) 0.0534(4) Uani 1 1 d . . . . .
O1 O 0.3920(3) 0.9150(4) 0.1943(6) 0.061(2) Uani 1 1 d . . . . .
O2 O 0.4487(3) 0.8590(3) 0.5666(6) 0.0496(17) Uani 1 1 d . . . . .
O3 O 0.4493(2) 0.6111(3) 0.5839(4) 0.0340(14) Uani 1 1 d . . . . .
O4 O 0.6458(2) 0.7291(3) 0.5479(5) 0.0373(14) Uani 1 1 d . . . . .
O5 O 0.6037(2) 0.5619(3) 0.2802(4) 0.0388(15) Uani 1 1 d . . . . .
C1 C 0.4445(4) 0.9183(4) 0.2266(7) 0.040(2) Uani 1 1 d . . . . .
C2 C 0.4624(4) 0.9202(4) 0.3277(8) 0.041(2) Uani 1 1 d . . . . .
H2 H 0.435854 0.920868 0.381511 0.049 Uiso 1 1 calc R . . . .
C3 C 0.5168(4) 0.9211(4) 0.3555(7) 0.033(2) Uani 1 1 d . . . . .
C4 C 0.5346(4) 0.9226(4) 0.4676(7) 0.040(2) Uani 1 1 d . . . . .
H4A H 0.507066 0.946478 0.508786 0.048 Uiso 1 1 calc R . . . .
H4B H 0.569635 0.946222 0.472803 0.048 Uiso 1 1 calc R . . . .
C5 C 0.5418(4) 0.8564(4) 0.5141(7) 0.034(2) Uani 1 1 d . . . . .
C6 C 0.4979(4) 0.8259(4) 0.5636(6) 0.0320(19) Uani 1 1 d . . . . .
C7 C 0.5026(4) 0.7627(4) 0.5995(6) 0.0311(19) Uani 1 1 d . . . . .
H7 H 0.472008 0.742120 0.630583 0.037 Uiso 1 1 calc R . . . .
C8 C 0.5514(3) 0.7300(4) 0.5899(6) 0.0265(17) Uani 1 1 d . . . . .
C9 C 0.5968(4) 0.7620(4) 0.5486(6) 0.0314(19) Uani 1 1 d . . . . .
C10 C 0.5909(4) 0.8235(4) 0.5081(7) 0.036(2) Uani 1 1 d . . . . .
H10 H 0.621279 0.843596 0.475576 0.043 Uiso 1 1 calc R . . . .
C11 C 0.5557(4) 0.6599(4) 0.6200(6) 0.0289(18) Uani 1 1 d . . . . .
H11A H 0.530616 0.650449 0.678434 0.035 Uiso 1 1 calc R . . . .
H11B H 0.593468 0.649945 0.642531 0.035 Uiso 1 1 calc R . . . .
C12 C 0.5406(3) 0.6191(4) 0.5255(6) 0.0268(18) Uani 1 1 d . . . . .
C13 C 0.5798(4) 0.6069(4) 0.4499(7) 0.0317(19) Uani 1 1 d . . . . .
H13 H 0.616060 0.621803 0.460376 0.038 Uiso 1 1 calc R . . . .
C14 C 0.5673(4) 0.5735(4) 0.3591(6) 0.0314(19) Uani 1 1 d . . . . .
C15 C 0.5144(4) 0.5486(4) 0.3452(6) 0.0294(18) Uani 1 1 d . . . . .
C16 C 0.4754(3) 0.5603(3) 0.4200(6) 0.0263(18) Uani 1 1 d . . . . .
H16 H 0.439480 0.543764 0.410840 0.032 Uiso 1 1 calc R . . . .
C17 C 0.4876(4) 0.5961(4) 0.5092(6) 0.0303(19) Uani 1 1 d . . . . .
C18 C 0.500000 0.5080(5) 0.250000 0.029(3) Uani 1 2 d S T P . .
H18A H 0.531409 0.479923 0.232780 0.035 Uiso 0.5 1 calc R . . . .
H18B H 0.468589 0.479926 0.267219 0.035 Uiso 0.5 1 calc R . . . .
C19 C 0.3497(4) 0.9104(6) 0.2702(9) 0.052(3) Uani 1 1 d . . . . .
H19A H 0.345416 0.951990 0.306814 0.063 Uiso 1 1 calc R . . . .
H19B H 0.358960 0.876968 0.322164 0.063 Uiso 1 1 calc R . . . .
C20 C 0.2963(4) 0.8927(6) 0.2144(8) 0.054(3) Uani 1 1 d . . . . .
H20A H 0.265495 0.896233 0.263929 0.065 Uiso 1 1 calc R . . . .
H20B H 0.298350 0.847396 0.190630 0.065 Uiso 1 1 calc R . . . .
C21 C 0.4199(6) 0.8573(6) 0.6634(10) 0.073(4) Uani 1 1 d . . . . .
H21A H 0.397769 0.817460 0.667082 0.088 Uiso 1 1 calc R . . . .
H21B H 0.446449 0.856547 0.721433 0.088 Uiso 1 1 calc R . . . .
C22 C 0.3856(7) 0.9108(7) 0.6740(12) 0.098(6) Uani 1 1 d . . . . .
H22A H 0.360886 0.912536 0.613133 0.118 Uiso 1 1 calc R . . . .
H22B H 0.408394 0.950181 0.672740 0.118 Uiso 1 1 calc R . . . .
C23 C 0.3956(4) 0.5857(4) 0.5676(7) 0.037(2) Uani 1 1 d . . . . .
H23A H 0.397078 0.538181 0.563782 0.044 Uiso 1 1 calc R . . . .
H23B H 0.380489 0.602155 0.501230 0.044 Uiso 1 1 calc R . . . .
C24 C 0.3601(4) 0.6063(5) 0.6565(8) 0.048(2) Uani 1 1 d . . . . .
H24A H 0.378911 0.596132 0.722675 0.057 Uiso 1 1 calc R . . . .
H24B H 0.325694 0.581114 0.654652 0.057 Uiso 1 1 calc R . . . .
C25 C 0.6945(4) 0.7629(5) 0.5246(10) 0.052(3) Uani 1 1 d . . . . .
H25A H 0.692539 0.806583 0.554983 0.062 Uiso 1 1 calc R . . . .
H25B H 0.697948 0.767461 0.448176 0.062 Uiso 1 1 calc R . . . .
C26 C 0.7430(4) 0.7297(5) 0.5652(9) 0.052(3) Uani 1 1 d . . . . .
H26A H 0.738855 0.723284 0.641083 0.062 Uiso 1 1 calc R . . . .
H26B H 0.775664 0.756956 0.553632 0.062 Uiso 1 1 calc R . . . .
C27 C 0.6591(4) 0.5819(5) 0.2964(7) 0.043(2) Uani 1 1 d . . . . .
H27A H 0.677494 0.552026 0.344996 0.052 Uiso 1 1 calc R . . . .
H27B H 0.659792 0.625597 0.327212 0.052 Uiso 1 1 calc R . . . .
C28 C 0.6879(4) 0.5822(5) 0.1946(8) 0.047(2) Uani 1 1 d . . . . .
H28A H 0.725702 0.597882 0.205099 0.057 Uiso 1 1 calc R . . . .
H28B H 0.669213 0.612536 0.147155 0.057 Uiso 1 1 calc R . . . .
O6 O 0.5246(7) 0.7398(8) 0.2702(16) 0.088(4) Uani 0.5 1 d D U . A -1
C29 C 0.6249(8) 0.7418(9) 0.2756(17) 0.060(4) Uani 0.5 1 d D U . A -1
H29B H 0.654301 0.725133 0.231385 0.090 Uiso 0.5 1 calc GR . . A -1
H29A H 0.621828 0.715203 0.338253 0.090 Uiso 0.5 1 calc GR . . A -1
H29C H 0.633233 0.786296 0.295552 0.090 Uiso 0.5 1 calc GR . . A -1
C30 C 0.5756(8) 0.7402(6) 0.2210(17) 0.083(4) Uani 0.5 1 d D U . A -1
C31 C 0.5714(11) 0.7380(12) 0.1135(17) 0.088(4) Uani 0.5 1 d D U . A -1
H31 H 0.600942 0.735730 0.065647 0.105 Uiso 0.5 1 calc R . . A -1
C32 C 0.5156(10) 0.7399(13) 0.0883(17) 0.095(4) Uani 0.5 1 d D U . A -1
H32 H 0.500531 0.740840 0.020203 0.114 Uiso 0.5 1 calc R . . A -1
C33 C 0.4859(11) 0.7400(13) 0.1836(19) 0.093(4) Uani 0.5 1 d D U . A -1
H33 H 0.447168 0.740205 0.189801 0.112 Uiso 0.5 1 calc R . . A -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0148 0.0070 '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'
Br Br -0.9502 1.0410 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0412 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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 O1 C19 118.9(8) . . ?
C6 O2 C21 116.1(8) . . ?
C17 O3 C23 116.0(6) . . ?
C9 O4 C25 119.2(7) . . ?
C14 O5 C27 117.1(7) . . ?
O1 C1 C2 126.5(9) . . ?
O1 C1 C3 114.1(8) . 3_655 ?
C2 C1 C3 119.3(9) . 3_655 ?
C1 C2 H2 118.2 . . ?
C1 C2 C3 123.7(9) . . ?
C3 C2 H2 118.2 . . ?
C1 C3 C4 121.3(8) 3_655 . ?
C2 C3 C1 116.8(8) . 3_655 ?
C2 C3 C4 121.9(9) . . ?
C3 C4 H4A 108.9 . . ?
C3 C4 H4B 108.9 . . ?
C3 C4 C5 113.2(7) . . ?
H4A C4 H4B 107.8 . . ?
C5 C4 H4A 108.9 . . ?
C5 C4 H4B 108.9 . . ?
C6 C5 C4 120.2(8) . . ?
C10 C5 C4 121.9(9) . . ?
C10 C5 C6 117.9(8) . . ?
O2 C6 C5 117.0(7) . . ?
O2 C6 C7 121.9(8) . . ?
C7 C6 C5 120.8(8) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 C6 120.3(8) . . ?
C8 C7 H7 119.8 . . ?
C7 C8 C9 119.1(7) . . ?
C7 C8 C11 120.9(7) . . ?
C9 C8 C11 120.0(7) . . ?
O4 C9 C8 117.2(7) . . ?
O4 C9 C10 122.9(8) . . ?
C10 C9 C8 119.9(8) . . ?
C5 C10 C9 121.6(9) . . ?
C5 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
C8 C11 H11A 110.0 . . ?
C8 C11 H11B 110.0 . . ?
C8 C11 C12 108.4(6) . . ?
H11A C11 H11B 108.4 . . ?
C12 C11 H11A 110.0 . . ?
C12 C11 H11B 110.0 . . ?
C13 C12 C11 119.4(7) . . ?
C13 C12 C17 118.2(7) . . ?
C17 C12 C11 122.3(7) . . ?
C12 C13 H13 119.1 . . ?
C12 C13 C14 121.8(8) . . ?
C14 C13 H13 119.1 . . ?
O5 C14 C13 124.4(8) . . ?
O5 C14 C15 116.0(7) . . ?
C13 C14 C15 119.5(8) . . ?
C14 C15 C18 121.2(7) . . ?
C16 C15 C14 119.0(7) . . ?
C16 C15 C18 119.8(7) . . ?
C15 C16 H16 119.4 . . ?
C15 C16 C17 121.1(8) . . ?
C17 C16 H16 119.4 . . ?
O3 C17 C12 116.7(7) . . ?
O3 C17 C16 123.0(8) . . ?
C12 C17 C16 120.3(8) . . ?
C15 C18 C15 113.0(9) 3_655 . ?
C15 C18 H18A 109.0 3_655 . ?
C15 C18 H18A 109.0 . . ?
C15 C18 H18B 109.0 3_655 . ?
C15 C18 H18B 109.0 . . ?
H18A C18 H18B 107.8 . . ?
O1 C19 H19A 110.0 . . ?
O1 C19 H19B 110.0 . . ?
O1 C19 C20 108.3(9) . . ?
H19A C19 H19B 108.4 . . ?
C20 C19 H19A 110.0 . . ?
C20 C19 H19B 110.0 . . ?
Br1 C20 H20A 109.3 . . ?
Br1 C20 H20B 109.3 . . ?
C19 C20 Br1 111.8(7) . . ?
C19 C20 H20A 109.3 . . ?
C19 C20 H20B 109.3 . . ?
H20A C20 H20B 107.9 . . ?
O2 C21 H21A 109.4 . . ?
O2 C21 H21B 109.4 . . ?
H21A C21 H21B 108.0 . . ?
C22 C21 O2 111.1(10) . . ?
C22 C21 H21A 109.4 . . ?
C22 C21 H21B 109.4 . . ?
Br2 C22 H22A 108.5 . . ?
Br2 C22 H22B 108.5 . . ?
C21 C22 Br2 115.0(9) . . ?
C21 C22 H22A 108.5 . . ?
C21 C22 H22B 108.5 . . ?
H22A C22 H22B 107.5 . . ?
O3 C23 H23A 110.0 . . ?
O3 C23 H23B 110.0 . . ?
O3 C23 C24 108.4(7) . . ?
H23A C23 H23B 108.4 . . ?
C24 C23 H23A 110.0 . . ?
C24 C23 H23B 110.0 . . ?
Br3 C24 H24A 108.9 . . ?
Br3 C24 H24B 108.9 . . ?
C23 C24 Br3 113.3(7) . . ?
C23 C24 H24A 108.9 . . ?
C23 C24 H24B 108.9 . . ?
H24A C24 H24B 107.7 . . ?
O4 C25 H25A 109.2 . . ?
O4 C25 H25B 109.2 . . ?
O4 C25 C26 111.9(8) . . ?
H25A C25 H25B 107.9 . . ?
C26 C25 H25A 109.2 . . ?
C26 C25 H25B 109.2 . . ?
Br4 C26 H26A 109.3 . . ?
Br4 C26 H26B 109.3 . . ?
C25 C26 Br4 111.6(8) . . ?
C25 C26 H26A 109.3 . . ?
C25 C26 H26B 109.3 . . ?
H26A C26 H26B 108.0 . . ?
O5 C27 H27A 109.9 . . ?
O5 C27 H27B 109.9 . . ?
O5 C27 C28 108.8(8) . . ?
H27A C27 H27B 108.3 . . ?
C28 C27 H27A 109.9 . . ?
C28 C27 H27B 109.9 . . ?
Br5 C28 H28A 109.0 . . ?
Br5 C28 H28B 109.0 . . ?
C27 C28 Br5 113.1(7) . . ?
C27 C28 H28A 109.0 . . ?
C27 C28 H28B 109.0 . . ?
H28A C28 H28B 107.8 . . ?
C30 O6 C33 103.6(17) . . ?
H29B C29 H29A 109.5 . . ?
H29B C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
C30 C29 H29B 109.5 . . ?
C30 C29 H29A 109.5 . . ?
C30 C29 H29C 109.5 . . ?
C29 C30 O6 122.9(16) . . ?
C31 C30 O6 113(2) . . ?
C31 C30 C29 124.5(16) . . ?
C30 C31 H31 126.2 . . ?
C30 C31 C32 108(2) . . ?
C32 C31 H31 126.2 . . ?
C31 C32 H32 126.3 . . ?
C31 C32 C33 107.4(19) . . ?
C33 C32 H32 126.3 . . ?
O6 C33 H33 125.6 . . ?
C32 C33 O6 108.8(17) . . ?
C32 C33 H33 125.6 . . ?
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
Br1 C20 1.944(10) . ?
Br2 C22 1.883(12) . ?
Br3 C24 1.915(11) . ?
Br4 C26 1.952(11) . ?
Br5 C28 1.947(10) . ?
O1 C1 1.353(12) . ?
O1 C19 1.425(12) . ?
O2 C6 1.388(11) . ?
O2 C21 1.430(13) . ?
O3 C17 1.379(10) . ?
O3 C23 1.431(11) . ?
O4 C9 1.380(10) . ?
O4 C25 1.416(11) . ?
O5 C14 1.371(10) . ?
O5 C27 1.433(11) . ?
C1 C2 1.372(14) . ?
C1 C3 1.418(13) 3_655 ?
C2 H2 0.9500 . ?
C2 C3 1.378(14) . ?
C3 C4 1.506(13) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.510(12) . ?
C5 C6 1.399(13) . ?
C5 C10 1.383(13) . ?
C6 C7 1.396(11) . ?
C7 H7 0.9500 . ?
C7 C8 1.379(12) . ?
C8 C9 1.399(12) . ?
C8 C11 1.510(11) . ?
C9 C10 1.388(12) . ?
C10 H10 0.9500 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.527(11) . ?
C12 C13 1.389(12) . ?
C12 C17 1.397(12) . ?
C13 H13 0.9500 . ?
C13 C14 1.392(12) . ?
C14 C15 1.405(12) . ?
C15 C16 1.377(12) . ?
C15 C18 1.527(10) . ?
C16 H16 0.9500 . ?
C16 C17 1.400(11) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.534(15) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.399(15) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.499(14) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.468(14) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.487(14) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
O6 C30 1.400(18) . ?
O6 C33 1.462(13) . ?
C29 H29B 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29C 0.9800 . ?
C29 C30 1.396(18) . ?
C30 C31 1.386(14) . ?
C31 H31 0.9500 . ?
C31 C32 1.404(18) . ?
C32 H32 0.9500 . ?
C32 C33 1.426(19) . ?
C33 H33 0.9500 . ?
