#------------------------------------------------------------------------------
#$Date: 2024-06-29 03:12:15 +0200 (Sat 29 de Jun de 2024) $
#$Revision: 292654 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/89/7248912.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_7248912
loop_
_publ_author_name
'Vinodh, Mickey'
'Alshammari, Anwar A.'
'Al-Azemi, Talal F.'
_publ_section_title
;
 Influence of halogen--halogen interactions in the self-assembly of
 pillar[5]arene-based supramolecular polymers
;
_journal_issue                   29
_journal_name_full               'RSC Advances'
_journal_page_first              20553
_journal_page_last               20560
_journal_paper_doi               10.1039/D4RA03769C
_journal_volume                  14
_journal_year                    2024
_chemical_formula_sum            'C53 H66 Br4 O10'
_chemical_formula_weight         1182.69
_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   geom
_audit_block_doi                 10.5517/ccdc.csd.cc243xnv
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2019-12-04 deposited with the CCDC.	2024-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                91.283(6)
_cell_angle_beta                 95.977(7)
_cell_angle_gamma                110.754(8)
_cell_formula_units_Z            2
_cell_length_a                   10.3567(8)
_cell_length_b                   12.1184(9)
_cell_length_c                   22.4299(15)
_cell_measurement_reflns_used    10746
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      3.19
_cell_volume                     2612.8(4)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0867
_diffrn_reflns_av_unetI/netI     0.1598
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            18256
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.028
_diffrn_reflns_theta_max         25.028
_diffrn_reflns_theta_min         3.186
_exptl_absorpt_coefficient_mu    3.137
_exptl_absorpt_correction_T_max  0.882
_exptl_absorpt_correction_T_min  0.388
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.162
_refine_diff_density_min         -1.102
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.905
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         9072
_refine_ls_number_restraints     577
_refine_ls_restrained_S_all      0.895
_refine_ls_R_factor_all          0.1513
_refine_ls_R_factor_gt           0.0653
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0878P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1549
_refine_ls_wR_factor_ref         0.1790
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4246
_reflns_number_total             9072
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ra03769c2.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        2612.8(3)
_cod_database_code               7248912
_shelx_shelxl_version_number     2017/1
_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_min   0.508
_shelx_estimated_absorpt_t_max   0.885
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
Br1 Br 0.03496(7) 0.52977(9) 0.74853(4) 0.0645(3) Uani 1 1 d . U . . .
Br2 Br 0.69164(8) 0.48852(10) 0.74255(4) 0.0799(4) Uani 1 1 d . U . . .
Br3 Br 0.21204(9) 0.89468(9) 1.04855(4) 0.0695(3) Uani 1 1 d . U . . .
Br4 Br 0.32649(9) 1.00386(10) 0.46489(5) 0.0881(4) Uani 1 1 d . U . . .
O1 O -0.0952(4) 0.1433(4) 0.73969(17) 0.0344(11) Uani 1 1 d . U . . .
O2 O 0.4173(4) 0.2318(5) 0.87097(19) 0.0426(12) Uani 1 1 d . U . . .
O3 O 0.0423(4) 0.4157(4) 0.92908(19) 0.0406(12) Uani 1 1 d . U . . .
O4 O 0.5998(4) 0.6793(4) 0.92769(18) 0.0371(11) Uani 1 1 d . U . . .
O5 O 0.1906(4) 0.8377(4) 0.86374(18) 0.0389(12) Uani 1 1 d . U . . .
O6 O 0.6471(4) 0.8978(4) 0.74256(18) 0.0351(11) Uani 1 1 d . U . . .
O7 O 0.1386(4) 0.8166(4) 0.63669(18) 0.0331(11) Uani 1 1 d . U . . .
O8 O 0.5003(4) 0.6061(4) 0.56893(19) 0.0397(12) Uani 1 1 d . U . . .
O9 O -0.0348(4) 0.3908(4) 0.57142(18) 0.0349(11) Uani 1 1 d . U . . .
O10 O 0.3552(4) 0.1840(4) 0.6322(2) 0.0417(12) Uani 1 1 d . U . . .
C1 C 0.1312(6) 0.1390(6) 0.7456(3) 0.0260(13) Uani 1 1 d . U . . .
C2 C 0.0309(5) 0.1658(6) 0.7743(3) 0.0279(13) Uani 1 1 d . U . . .
C3 C 0.0611(6) 0.2123(6) 0.8321(3) 0.0283(14) Uani 1 1 d . U . . .
H3 H -0.008336 0.230001 0.850602 0.034 Uiso 1 1 calc R U . . .
C4 C 0.1893(6) 0.2345(6) 0.8647(3) 0.0293(13) Uani 1 1 d . U . . .
C5 C 0.2884(6) 0.2046(6) 0.8364(3) 0.0308(14) Uani 1 1 d . U . . .
C6 C 0.2602(6) 0.1606(6) 0.7783(3) 0.0282(14) Uani 1 1 d . U . . .
H6 H 0.330248 0.144305 0.759560 0.034 Uiso 1 1 calc R U . . .
C7 C 0.2214(6) 0.2901(6) 0.9287(3) 0.0336(14) Uani 1 1 d . U . . .
H7A H 0.136445 0.261641 0.949220 0.040 Uiso 1 1 calc R U . . .
H7B H 0.293263 0.265788 0.951275 0.040 Uiso 1 1 calc R U . . .
C8 C 0.2723(6) 0.4226(6) 0.9285(2) 0.0298(13) Uani 1 1 d . U . . .
C9 C 0.1803(6) 0.4864(6) 0.9291(3) 0.0303(13) Uani 1 1 d . U . . .
C10 C 0.2294(6) 0.6072(6) 0.9300(3) 0.0319(14) Uani 1 1 d . U . . .
H10 H 0.165819 0.647536 0.930646 0.038 Uiso 1 1 calc R U . . .
C11 C 0.3709(6) 0.6726(6) 0.9299(3) 0.0312(13) Uani 1 1 d . U . . .
C12 C 0.4600(6) 0.6101(7) 0.9285(3) 0.0326(14) Uani 1 1 d . U . . .
C13 C 0.4124(6) 0.4873(6) 0.9277(2) 0.0311(14) Uani 1 1 d . U . . .
H13 H 0.476336 0.447445 0.926512 0.037 Uiso 1 1 calc R U . . .
C14 C 0.4203(6) 0.8051(6) 0.9282(3) 0.0366(15) Uani 1 1 d . U . . .
H14A H 0.515440 0.840394 0.949665 0.044 Uiso 1 1 calc R U . . .
H14B H 0.358593 0.835256 0.949046 0.044 Uiso 1 1 calc R U . . .
C15 C 0.4206(6) 0.8421(6) 0.8643(3) 0.0302(14) Uani 1 1 d . U . . .
C16 C 0.3042(6) 0.8567(6) 0.8327(3) 0.0319(14) Uani 1 1 d . U . . .
C17 C 0.3073(6) 0.8884(6) 0.7734(3) 0.0286(14) Uani 1 1 d . U . . .
H17 H 0.228978 0.900633 0.752933 0.034 Uiso 1 1 calc R U . . .
C18 C 0.4212(6) 0.9022(6) 0.7439(3) 0.0291(13) Uani 1 1 d . U . . .
C19 C 0.5366(6) 0.8852(6) 0.7749(3) 0.0295(14) Uani 1 1 d . U . . .
C20 C 0.5357(6) 0.8579(6) 0.8339(3) 0.0270(14) Uani 1 1 d . U . . .
H20 H 0.616187 0.849503 0.854649 0.032 Uiso 1 1 calc R U . . .
C21 C 0.4192(6) 0.9296(6) 0.6779(3) 0.0290(13) Uani 1 1 d . U . . .
H21A H 0.359055 0.976421 0.668967 0.035 Uiso 1 1 calc R U . . .
H21B H 0.514501 0.977984 0.669954 0.035 Uiso 1 1 calc R U . . .
C22 C 0.3669(5) 0.8197(6) 0.6374(3) 0.0266(13) Uani 1 1 d . U . . .
C23 C 0.2259(6) 0.7611(6) 0.6179(3) 0.0257(13) Uani 1 1 d . U . . .
C24 C 0.1806(6) 0.6587(6) 0.5821(3) 0.0277(13) Uani 1 1 d . U . . .
H24 H 0.084254 0.622738 0.568224 0.033 Uiso 1 1 calc R U . . .
C25 C 0.2723(6) 0.6056(6) 0.5652(2) 0.0268(13) Uani 1 1 d . U . . .
C26 C 0.4137(6) 0.6633(6) 0.5860(3) 0.0289(13) Uani 1 1 d . U . . .
C27 C 0.4580(6) 0.7676(6) 0.6204(3) 0.0281(13) Uani 1 1 d . U . . .
H27 H 0.554564 0.805507 0.633126 0.034 Uiso 1 1 calc R U . . .
C28 C 0.2207(6) 0.4918(6) 0.5280(2) 0.0279(13) Uani 1 1 d . U . . .
H28A H 0.291862 0.490915 0.501988 0.033 Uiso 1 1 calc R U . . .
H28B H 0.135595 0.486576 0.501676 0.033 Uiso 1 1 calc R U . . .
C29 C 0.1885(6) 0.3859(6) 0.5651(2) 0.0278(13) Uani 1 1 d . U . . .
C30 C 0.0596(5) 0.3362(6) 0.5871(3) 0.0273(13) Uani 1 1 d . U . . .
C31 C 0.0337(5) 0.2403(6) 0.6225(2) 0.0268(14) Uani 1 1 d . U . . .
H31 H -0.054778 0.207936 0.636556 0.032 Uiso 1 1 calc R U . . .
C32 C 0.1322(6) 0.1904(6) 0.6381(3) 0.0254(13) Uani 1 1 d . U . . .
C33 C 0.2601(6) 0.2378(6) 0.6163(3) 0.0293(13) Uani 1 1 d . U . . .
C34 C 0.2858(6) 0.3307(6) 0.5797(3) 0.0297(14) Uani 1 1 d . U . . .
H34 H 0.372124 0.358744 0.563543 0.036 Uiso 1 1 calc R U . . .
C35 C 0.1012(6) 0.0912(6) 0.6806(3) 0.0305(14) Uani 1 1 d . U . . .
H35A H 0.158681 0.042952 0.673801 0.037 Uiso 1 1 calc R U . . .
H35B H 0.002208 0.039311 0.672036 0.037 Uiso 1 1 calc R U . . .
C36 C -0.1951(6) 0.1796(7) 0.7657(3) 0.0419(18) Uani 1 1 d . U . . .
H36A H -0.227873 0.130733 0.799199 0.050 Uiso 1 1 calc R U . . .
H36B H -0.274036 0.170118 0.735287 0.050 Uiso 1 1 calc R U . . .
H36C H -0.152056 0.262759 0.780480 0.050 Uiso 1 1 calc R U . . .
C37 C 0.5161(7) 0.1918(8) 0.8468(3) 0.057(2) Uani 1 1 d . U . . .
H37A H 0.601707 0.215826 0.874890 0.069 Uiso 1 1 calc R U . . .
H37B H 0.536762 0.226722 0.808335 0.069 Uiso 1 1 calc R U . . .
H37C H 0.477705 0.105433 0.840603 0.069 Uiso 1 1 calc R U . . .
C38 C -0.0562(6) 0.4728(7) 0.9196(3) 0.0451(19) Uani 1 1 d . U . . .
H38A H -0.150453 0.413946 0.917693 0.054 Uiso 1 1 calc R U . . .
H38B H -0.045121 0.512061 0.881739 0.054 Uiso 1 1 calc R U . . .
H38C H -0.040729 0.531638 0.952827 0.054 Uiso 1 1 calc R U . . .
C39 C 0.6924(6) 0.6196(7) 0.9175(3) 0.0407(18) Uani 1 1 d . U . . .
H39A H 0.689954 0.563761 0.948702 0.049 Uiso 1 1 calc R U . . .
H39B H 0.787149 0.677398 0.918745 0.049 Uiso 1 1 calc R U . . .
H39C H 0.663975 0.576385 0.878012 0.049 Uiso 1 1 calc R U . . .
C40 C 0.0677(6) 0.8420(8) 0.8311(3) 0.047(2) Uani 1 1 d . U . . .
H40A H 0.037529 0.782604 0.797148 0.057 Uiso 1 1 calc R U . . .
H40B H 0.086458 0.920761 0.816001 0.057 Uiso 1 1 calc R U . . .
H40C H -0.005686 0.825498 0.857477 0.057 Uiso 1 1 calc R U . . .
C41 C 0.7631(6) 0.8768(7) 0.7722(3) 0.0424(19) Uani 1 1 d . U . . .
H41A H 0.838650 0.898507 0.746760 0.051 Uiso 1 1 calc R U . . .
H41B H 0.736292 0.792803 0.779887 0.051 Uiso 1 1 calc R U . . .
H41C H 0.794518 0.924494 0.810365 0.051 Uiso 1 1 calc R U . . .
C42 C -0.0068(6) 0.7534(7) 0.6236(3) 0.0391(17) Uani 1 1 d . U . . .
H42A H -0.029501 0.673625 0.637903 0.047 Uiso 1 1 calc R U . . .
H42B H -0.033564 0.748076 0.580161 0.047 Uiso 1 1 calc R U . . .
H42C H -0.057488 0.794851 0.643861 0.047 Uiso 1 1 calc R U . . .
C43 C 0.6431(6) 0.6630(7) 0.5912(3) 0.047(2) Uani 1 1 d . U . . .
H43A H 0.695655 0.614770 0.579094 0.057 Uiso 1 1 calc R U . . .
H43B H 0.653009 0.672700 0.635088 0.057 Uiso 1 1 calc R U . . .
H43C H 0.679035 0.740781 0.574627 0.057 Uiso 1 1 calc R U . . .
C44 C -0.1642(6) 0.3469(7) 0.5954(3) 0.044(2) Uani 1 1 d . U . . .
H44A H -0.222214 0.391823 0.580950 0.053 Uiso 1 1 calc R U . . .
H44B H -0.147692 0.355486 0.639341 0.053 Uiso 1 1 calc R U . . .
H44C H -0.211943 0.263192 0.582314 0.053 Uiso 1 1 calc R U . . .
C45 C 0.4836(6) 0.2259(7) 0.6069(4) 0.052(2) Uani 1 1 d . U . . .
H45A H 0.537414 0.175683 0.617892 0.063 Uiso 1 1 calc R U . . .
H45B H 0.536811 0.307482 0.622341 0.063 Uiso 1 1 calc R U . . .
H45C H 0.464654 0.223272 0.563035 0.063 Uiso 1 1 calc R U . . .
C46 C 0.2330(9) 0.5792(10) 0.7582(5) 0.107(3) Uani 1 1 d D U . . .
H46A H 0.271372 0.648259 0.734087 0.128 Uiso 1 1 calc R U . . .
H46B H 0.268437 0.604695 0.800906 0.128 Uiso 1 1 calc R U . . .
C47 C 0.2827(7) 0.4855(9) 0.7398(5) 0.097(3) Uani 1 1 d D U . . .
H47A H 0.250515 0.460306 0.696836 0.117 Uiso 1 1 calc R U . . .
H47B H 0.246611 0.416003 0.763868 0.117 Uiso 1 1 calc R U . . .
C48 C 0.4434(7) 0.5375(9) 0.7504(5) 0.089(3) Uani 1 1 d D U . . .
H48A H 0.479931 0.605276 0.725275 0.107 Uiso 1 1 calc R U . . .
H48B H 0.475853 0.564860 0.793100 0.107 Uiso 1 1 calc R U . . .
C49 C 0.4911(9) 0.4401(10) 0.7334(6) 0.124(3) Uani 1 1 d D U . . .
H49A H 0.454456 0.412116 0.691009 0.148 Uiso 1 1 calc R U . . .
H49B H 0.452493 0.373058 0.758689 0.148 Uiso 1 1 calc R U . . .
C50 C 0.1844(7) 1.0000(7) 0.9889(3) 0.0496(19) Uani 1 1 d . U . . .
H50A H 0.238087 1.082806 1.003892 0.059 Uiso 1 1 calc R U . . .
H50B H 0.220459 0.984565 0.951652 0.059 Uiso 1 1 calc R U . . .
C51 C 0.0319(7) 0.9843(7) 0.9746(3) 0.0447(18) Uani 1 1 d . U . . .
H51A H 0.022836 1.033509 0.940958 0.054 Uiso 1 1 calc R U . . .
H51B H -0.021156 0.900682 0.960783 0.054 Uiso 1 1 calc R U . . .
C52 C 0.1620(7) 0.9555(8) 0.5057(3) 0.057(2) Uani 1 1 d . U . . .
H52A H 0.110669 0.869610 0.496973 0.068 Uiso 1 1 calc R U . . .
H52B H 0.189501 0.969858 0.549559 0.068 Uiso 1 1 calc R U . . .
C53 C 0.0675(7) 1.0226(7) 0.4858(3) 0.0457(18) Uani 1 1 d . U . . .
H53A H 0.046186 1.013580 0.441538 0.055 Uiso 1 1 calc R U . . .
H53B H 0.116097 1.107825 0.497533 0.055 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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D0PY00327A 2020
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 O1 C36 116.8(5) . . ?
C5 O2 C37 116.9(5) . . ?
C9 O3 C38 116.3(5) . . ?
C12 O4 C39 117.4(6) . . ?
C16 O5 C40 117.0(4) . . ?
C19 O6 C41 117.3(4) . . ?
C23 O7 C42 116.5(5) . . ?
C26 O8 C43 114.8(5) . . ?
C30 O9 C44 117.0(4) . . ?
C33 O10 C45 117.2(5) . . ?
C6 C1 C2 117.8(6) . . ?
C6 C1 C35 121.1(5) . . ?
C2 C1 C35 121.1(5) . . ?
C3 C2 O1 124.2(5) . . ?
C3 C2 C1 120.4(5) . . ?
O1 C2 C1 115.4(5) . . ?
C2 C3 C4 122.1(5) . . ?
C2 C3 H3 118.9 . . ?
C4 C3 H3 118.9 . . ?
C3 C4 C5 117.4(6) . . ?
C3 C4 C7 120.9(5) . . ?
C5 C4 C7 121.7(5) . . ?
C6 C5 O2 124.2(5) . . ?
C6 C5 C4 120.8(5) . . ?
O2 C5 C4 114.9(6) . . ?
C5 C6 C1 121.4(5) . . ?
C5 C6 H6 119.3 . . ?
C1 C6 H6 119.3 . . ?
C8 C7 C4 110.6(5) . . ?
C8 C7 H7A 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
C13 C8 C9 117.5(6) . . ?
C13 C8 C7 120.4(6) . . ?
C9 C8 C7 122.0(5) . . ?
C10 C9 O3 124.9(6) . . ?
C10 C9 C8 121.0(6) . . ?
O3 C9 C8 114.1(6) . . ?
C9 C10 C11 121.5(6) . . ?
C9 C10 H10 119.3 . . ?
C11 C10 H10 119.3 . . ?
C12 C11 C10 117.4(7) . . ?
C12 C11 C14 122.6(6) . . ?
C10 C11 C14 120.0(6) . . ?
C11 C12 C13 122.1(6) . . ?
C11 C12 O4 115.1(6) . . ?
C13 C12 O4 122.8(6) . . ?
C8 C13 C12 120.5(6) . . ?
C8 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C11 C14 C15 111.2(6) . . ?
C11 C14 H14A 109.4 . . ?
C15 C14 H14A 109.4 . . ?
C11 C14 H14B 109.4 . . ?
C15 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C20 C15 C16 117.6(5) . . ?
C20 C15 C14 120.5(5) . . ?
C16 C15 C14 121.8(5) . . ?
O5 C16 C17 123.7(5) . . ?
O5 C16 C15 116.1(5) . . ?
C17 C16 C15 120.1(5) . . ?
C18 C17 C16 121.4(5) . . ?
C18 C17 H17 119.3 . . ?
C16 C17 H17 119.3 . . ?
C17 C18 C19 118.6(5) . . ?
C17 C18 C21 120.6(5) . . ?
C19 C18 C21 120.7(5) . . ?
C20 C19 O6 123.7(5) . . ?
C20 C19 C18 120.2(5) . . ?
O6 C19 C18 116.1(5) . . ?
C19 C20 C15 122.0(5) . . ?
C19 C20 H20 119.0 . . ?
C15 C20 H20 119.0 . . ?
C22 C21 C18 111.8(5) . . ?
C22 C21 H21A 109.3 . . ?
C18 C21 H21A 109.3 . . ?
C22 C21 H21B 109.3 . . ?
C18 C21 H21B 109.3 . . ?
H21A C21 H21B 107.9 . . ?
C27 C22 C23 117.1(6) . . ?
C27 C22 C21 120.3(5) . . ?
C23 C22 C21 122.5(5) . . ?
C24 C23 C22 121.2(5) . . ?
C24 C23 O7 124.0(5) . . ?
C22 C23 O7 114.8(6) . . ?
C23 C24 C25 121.7(5) . . ?
C23 C24 H24 119.1 . . ?
C25 C24 H24 119.1 . . ?
C24 C25 C26 116.9(6) . . ?
C24 C25 C28 121.1(5) . . ?
C26 C25 C28 122.0(5) . . ?
C27 C26 O8 124.6(5) . . ?
C27 C26 C25 120.7(5) . . ?
O8 C26 C25 114.8(6) . . ?
C26 C27 C22 122.4(6) . . ?
C26 C27 H27 118.8 . . ?
C22 C27 H27 118.8 . . ?
C25 C28 C29 112.8(5) . . ?
C25 C28 H28A 109.0 . . ?
C29 C28 H28A 109.0 . . ?
C25 C28 H28B 109.0 . . ?
C29 C28 H28B 109.0 . . ?
H28A C28 H28B 107.8 . . ?
C30 C29 C34 116.4(5) . . ?
C30 C29 C28 121.8(5) . . ?
C34 C29 C28 121.9(5) . . ?
O9 C30 C31 124.1(5) . . ?
O9 C30 C29 115.2(5) . . ?
C31 C30 C29 120.7(5) . . ?
C32 C31 C30 122.0(5) . . ?
C32 C31 H31 119.0 . . ?
C30 C31 H31 119.0 . . ?
C31 C32 C33 118.1(5) . . ?
C31 C32 C35 119.5(5) . . ?
C33 C32 C35 122.3(5) . . ?
C34 C33 O10 123.2(5) . . ?
C34 C33 C32 120.5(5) . . ?
O10 C33 C32 116.3(5) . . ?
C33 C34 C29 122.2(5) . . ?
C33 C34 H34 118.9 . . ?
C29 C34 H34 118.9 . . ?
C32 C35 C1 111.4(6) . . ?
C32 C35 H35A 109.4 . . ?
C1 C35 H35A 109.4 . . ?
C32 C35 H35B 109.4 . . ?
C1 C35 H35B 109.4 . . ?
H35A C35 H35B 108.0 . . ?
O1 C36 H36A 109.5 . . ?
O1 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
O1 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O2 C37 H37A 109.5 . . ?
O2 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
O2 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O3 C38 H38A 109.5 . . ?
O3 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
O3 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O4 C39 H39A 109.5 . . ?
O4 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
O4 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O5 C40 H40A 109.5 . . ?
O5 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
O5 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
O6 C41 H41A 109.5 . . ?
O6 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
O6 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O7 C42 H42A 109.5 . . ?
O7 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
O7 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O8 C43 H43A 109.5 . . ?
O8 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
O8 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O9 C44 H44A 109.5 . . ?
O9 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
O9 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O10 C45 H45A 109.5 . . ?
O10 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
O10 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C47 C46 Br1 112.8(7) . . ?
C47 C46 H46A 109.0 . . ?
Br1 C46 H46A 109.0 . . ?
C47 C46 H46B 109.0 . . ?
Br1 C46 H46B 109.0 . . ?
H46A C46 H46B 107.8 . . ?
C46 C47 C48 107.1(8) . . ?
C46 C47 H47A 110.3 . . ?
C48 C47 H47A 110.3 . . ?
C46 C47 H47B 110.3 . . ?
C48 C47 H47B 110.3 . . ?
H47A C47 H47B 108.6 . . ?
C49 C48 C47 106.1(8) . . ?
C49 C48 H48A 110.5 . . ?
C47 C48 H48A 110.5 . . ?
C49 C48 H48B 110.5 . . ?
C47 C48 H48B 110.5 . . ?
H48A C48 H48B 108.7 . . ?
C48 C49 Br2 112.5(7) . . ?
C48 C49 H49A 109.1 . . ?
Br2 C49 H49A 109.1 . . ?
C48 C49 H49B 109.1 . . ?
Br2 C49 H49B 109.1 . . ?
H49A C49 H49B 107.8 . . ?
C51 C50 Br3 112.1(5) . . ?
C51 C50 H50A 109.2 . . ?
Br3 C50 H50A 109.2 . . ?
C51 C50 H50B 109.2 . . ?
Br3 C50 H50B 109.2 . . ?
H50A C50 H50B 107.9 . . ?
C51 C51 C50 114.9(7) 2_577 . ?
C51 C51 H51A 108.5 2_577 . ?
C50 C51 H51A 108.5 . . ?
C51 C51 H51B 108.5 2_577 . ?
C50 C51 H51B 108.5 . . ?
H51A C51 H51B 107.5 . . ?
C53 C52 Br4 111.3(5) . . ?
C53 C52 H52A 109.4 . . ?
Br4 C52 H52A 109.4 . . ?
C53 C52 H52B 109.4 . . ?
Br4 C52 H52B 109.4 . . ?
H52A C52 H52B 108.0 . . ?
C52 C53 C53 111.2(7) . 2_576 ?
C52 C53 H53A 109.4 . . ?
C53 C53 H53A 109.4 2_576 . ?
C52 C53 H53B 109.4 . . ?
C53 C53 H53B 109.4 2_576 . ?
H53A C53 H53B 108.0 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C46 1.909(8) . ?
Br2 C49 1.935(8) . ?
Br3 C50 1.938(7) . ?
Br4 C52 1.930(7) . ?
O1 C2 1.382(6) . ?
O1 C36 1.429(7) . ?
O2 C5 1.397(7) . ?
O2 C37 1.424(8) . ?
O3 C9 1.381(7) . ?
O3 C38 1.423(7) . ?
O4 C12 1.395(7) . ?
O4 C39 1.423(7) . ?
O5 C16 1.381(6) . ?
O5 C40 1.420(7) . ?
O6 C19 1.384(6) . ?
O6 C41 1.416(7) . ?
O7 C23 1.395(7) . ?
O7 C42 1.421(7) . ?
O8 C26 1.390(7) . ?
O8 C43 1.421(7) . ?
O9 C30 1.384(7) . ?
O9 C44 1.423(6) . ?
O10 C33 1.384(7) . ?
O10 C45 1.427(7) . ?
C1 C6 1.389(7) . ?
C1 C2 1.403(8) . ?
C1 C35 1.517(8) . ?
C2 C3 1.362(8) . ?
C3 C4 1.380(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.407(8) . ?
C4 C7 1.524(8) . ?
C5 C6 1.360(8) . ?
C6 H6 0.9500 . ?
C7 C8 1.502(9) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C13 1.386(8) . ?
C8 C9 1.424(8) . ?
C9 C10 1.368(9) . ?
C10 C11 1.397(8) . ?
C10 H10 0.9500 . ?
C11 C12 1.389(9) . ?
C11 C14 1.506(10) . ?
C12 C13 1.391(9) . ?
C13 H13 0.9500 . ?
C14 C15 1.510(8) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C20 1.392(8) . ?
C15 C16 1.402(8) . ?
C16 C17 1.393(8) . ?
C17 C18 1.373(8) . ?
C17 H17 0.9500 . ?
C18 C19 1.400(8) . ?
C18 C21 1.524(8) . ?
C19 C20 1.372(8) . ?
C20 H20 0.9500 . ?
C21 C22 1.491(9) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C27 1.386(8) . ?
C22 C23 1.395(8) . ?
C23 C24 1.368(9) . ?
C24 C25 1.398(8) . ?
C24 H24 0.9500 . ?
C25 C26 1.403(8) . ?
C25 C28 1.489(9) . ?
C26 C27 1.369(9) . ?
C27 H27 0.9500 . ?
C28 C29 1.502(8) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.402(7) . ?
C29 C34 1.410(8) . ?
C30 C31 1.385(8) . ?
C31 C32 1.380(8) . ?
C31 H31 0.9500 . ?
C32 C33 1.390(8) . ?
C32 C35 1.516(8) . ?
C33 C34 1.374(8) . ?
C34 H34 0.9500 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C47 1.471(8) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.546(8) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C49 1.489(8) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 C51 1.520(9) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C51 1.482(13) 2_577 ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 C53 1.519(10) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 C53 1.522(13) 2_576 ?
C53 H53A 0.9900 . ?
C53 H53B 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
C36 O1 C2 C3 4.6(9) . . . . ?
C36 O1 C2 C1 -174.5(5) . . . . ?
C6 C1 C2 C3 0.5(9) . . . . ?
C35 C1 C2 C3 -177.8(6) . . . . ?
C6 C1 C2 O1 179.6(5) . . . . ?
C35 C1 C2 O1 1.3(8) . . . . ?
O1 C2 C3 C4 -179.2(5) . . . . ?
C1 C2 C3 C4 -0.2(10) . . . . ?
C2 C3 C4 C5 -1.5(9) . . . . ?
C2 C3 C4 C7 178.1(6) . . . . ?
C37 O2 C5 C6 -11.2(9) . . . . ?
C37 O2 C5 C4 173.5(6) . . . . ?
C3 C4 C5 C6 2.9(9) . . . . ?
C7 C4 C5 C6 -176.6(6) . . . . ?
C3 C4 C5 O2 178.4(5) . . . . ?
C7 C4 C5 O2 -1.1(9) . . . . ?
O2 C5 C6 C1 -177.8(6) . . . . ?
C4 C5 C6 C1 -2.8(10) . . . . ?
C2 C1 C6 C5 1.0(9) . . . . ?
C35 C1 C6 C5 179.3(6) . . . . ?
C3 C4 C7 C8 -86.0(7) . . . . ?
C5 C4 C7 C8 93.6(7) . . . . ?
C4 C7 C8 C13 -87.6(6) . . . . ?
C4 C7 C8 C9 92.4(6) . . . . ?
C38 O3 C9 C10 10.4(8) . . . . ?
C38 O3 C9 C8 -169.9(5) . . . . ?
C13 C8 C9 C10 -1.2(8) . . . . ?
C7 C8 C9 C10 178.9(6) . . . . ?
C13 C8 C9 O3 179.1(5) . . . . ?
C7 C8 C9 O3 -0.9(8) . . . . ?
O3 C9 C10 C11 -179.9(5) . . . . ?
C8 C9 C10 C11 0.4(9) . . . . ?
C9 C10 C11 C12 0.3(9) . . . . ?
C9 C10 C11 C14 177.4(5) . . . . ?
C10 C11 C12 C13 -0.4(9) . . . . ?
C14 C11 C12 C13 -177.4(6) . . . . ?
C10 C11 C12 O4 179.2(5) . . . . ?
C14 C11 C12 O4 2.2(8) . . . . ?
C39 O4 C12 C11 -171.0(5) . . . . ?
C39 O4 C12 C13 8.5(8) . . . . ?
C9 C8 C13 C12 1.2(8) . . . . ?
C7 C8 C13 C12 -178.9(5) . . . . ?
C11 C12 C13 C8 -0.4(9) . . . . ?
O4 C12 C13 C8 -179.9(5) . . . . ?
C12 C11 C14 C15 87.1(7) . . . . ?
C10 C11 C14 C15 -89.8(7) . . . . ?
C11 C14 C15 C20 -87.0(7) . . . . ?
C11 C14 C15 C16 90.2(8) . . . . ?
C40 O5 C16 C17 5.1(10) . . . . ?
C40 O5 C16 C15 -174.8(6) . . . . ?
C20 C15 C16 O5 178.5(6) . . . . ?
C14 C15 C16 O5 1.3(10) . . . . ?
C20 C15 C16 C17 -1.4(10) . . . . ?
C14 C15 C16 C17 -178.6(6) . . . . ?
O5 C16 C17 C18 -177.7(6) . . . . ?
C15 C16 C17 C18 2.2(10) . . . . ?
C16 C17 C18 C19 -0.8(10) . . . . ?
C16 C17 C18 C21 176.3(6) . . . . ?
C41 O6 C19 C20 2.3(10) . . . . ?
C41 O6 C19 C18 -177.7(6) . . . . ?
C17 C18 C19 C20 -1.4(10) . . . . ?
C21 C18 C19 C20 -178.5(6) . . . . ?
C17 C18 C19 O6 178.6(6) . . . . ?
C21 C18 C19 O6 1.6(9) . . . . ?
O6 C19 C20 C15 -177.8(6) . . . . ?
C18 C19 C20 C15 2.2(10) . . . . ?
C16 C15 C20 C19 -0.8(10) . . . . ?
C14 C15 C20 C19 176.4(6) . . . . ?
C17 C18 C21 C22 -89.9(7) . . . . ?
C19 C18 C21 C22 87.1(7) . . . . ?
C18 C21 C22 C27 -88.3(6) . . . . ?
C18 C21 C22 C23 87.8(6) . . . . ?
C27 C22 C23 C24 -2.1(8) . . . . ?
C21 C22 C23 C24 -178.3(5) . . . . ?
C27 C22 C23 O7 179.4(5) . . . . ?
C21 C22 C23 O7 3.2(8) . . . . ?
C42 O7 C23 C24 8.4(8) . . . . ?
C42 O7 C23 C22 -173.1(5) . . . . ?
C22 C23 C24 C25 2.6(8) . . . . ?
O7 C23 C24 C25 -179.0(5) . . . . ?
C23 C24 C25 C26 -1.1(8) . . . . ?
C23 C24 C25 C28 177.7(5) . . . . ?
C43 O8 C26 C27 1.2(8) . . . . ?
C43 O8 C26 C25 -178.5(5) . . . . ?
C24 C25 C26 C27 -0.8(8) . . . . ?
C28 C25 C26 C27 -179.6(5) . . . . ?
C24 C25 C26 O8 178.9(5) . . . . ?
C28 C25 C26 O8 0.1(7) . . . . ?
O8 C26 C27 C22 -178.4(5) . . . . ?
C25 C26 C27 C22 1.3(8) . . . . ?
C23 C22 C27 C26 0.1(8) . . . . ?
C21 C22 C27 C26 176.5(5) . . . . ?
C24 C25 C28 C29 -91.2(6) . . . . ?
C26 C25 C28 C29 87.5(6) . . . . ?
C25 C28 C29 C30 84.9(7) . . . . ?
C25 C28 C29 C34 -95.3(7) . . . . ?
C44 O9 C30 C31 2.2(9) . . . . ?
C44 O9 C30 C29 -176.8(6) . . . . ?
C34 C29 C30 O9 -179.0(5) . . . . ?
C28 C29 C30 O9 0.8(9) . . . . ?
C34 C29 C30 C31 1.9(9) . . . . ?
C28 C29 C30 C31 -178.3(6) . . . . ?
O9 C30 C31 C32 -178.5(6) . . . . ?
C29 C30 C31 C32 0.5(10) . . . . ?
C30 C31 C32 C33 -1.0(10) . . . . ?
C30 C31 C32 C35 175.7(6) . . . . ?
C45 O10 C33 C34 -2.3(10) . . . . ?
C45 O10 C33 C32 175.7(6) . . . . ?
C31 C32 C33 C34 -0.9(10) . . . . ?
C35 C32 C33 C34 -177.6(6) . . . . ?
C31 C32 C33 O10 -179.0(5) . . . . ?
C35 C32 C33 O10 4.4(9) . . . . ?
O10 C33 C34 C29 -178.6(6) . . . . ?
C32 C33 C34 C29 3.5(10) . . . . ?
C30 C29 C34 C33 -3.9(9) . . . . ?
C28 C29 C34 C33 176.3(6) . . . . ?
C31 C32 C35 C1 -83.4(7) . . . . ?
C33 C32 C35 C1 93.1(7) . . . . ?
C6 C1 C35 C32 -92.1(7) . . . . ?
C2 C1 C35 C32 86.1(7) . . . . ?
Br1 C46 C47 C48 -179.7(7) . . . . ?
C46 C47 C48 C49 178.2(10) . . . . ?
C47 C48 C49 Br2 179.2(7) . . . . ?
Br3 C50 C51 C51 64.4(10) . . . 2_577 ?
Br4 C52 C53 C53 175.4(7) . . . 2_576 ?
