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#$Date: 2024-09-06 03:12:32 +0300 (Fri, 06 Sep 2024) $
#$Revision: 294503 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/91/7249138.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_7249138
loop_
_publ_author_name
'Kawahata, Masatoshi'
'Hyodo, Tadashi'
'Kondo, Rina'
'Tominaga, Masahide'
'Yamaguchi, Kentaro'
_publ_section_title
;
 Inclusion of halobenzene in water-mediated hydrogen-bonded architectures
 built from a V-shaped host molecule
;
_journal_issue                   32
_journal_name_full               CrystEngComm
_journal_page_first              4272
_journal_page_last               4277
_journal_paper_doi               10.1039/D4CE00616J
_journal_volume                  26
_journal_year                    2024
_chemical_formula_sum            'C32 H38 Cl2 O7'
_chemical_formula_weight         605.52
_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   mixed
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-05-18 deposited with the CCDC.	2024-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                111.592(4)
_cell_angle_beta                 103.293(4)
_cell_angle_gamma                98.851(4)
_cell_formula_units_Z            2
_cell_length_a                   9.710(4)
_cell_length_b                   13.163(5)
_cell_length_c                   13.202(5)
_cell_measurement_reflns_used    6866
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.82
_cell_measurement_theta_min      2.21
_cell_volume                     1473.0(10)
_computing_cell_refinement       'SAINT (Bruker AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXLE (Hübschle et al., 2011)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13482
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.057
_diffrn_reflns_theta_min         1.725
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.268
_exptl_absorpt_correction_T_max  0.9583
_exptl_absorpt_correction_T_min  0.8450
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         5250
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0506
_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)+(0.0545P)²+1.3920P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1358
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3811
_reflns_number_total             5250
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ce00616j2.cif
_cod_data_source_block           1d
_cod_depositor_comments
'Adding full bibliography for 7249135--7249139.cif.'
_cod_database_code               7249138
_shelx_shelxl_version_number     2019/3
_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   0.924
_shelx_estimated_absorpt_t_max   0.948
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 0.1174(3) 0.2095(2) 0.7962(2) 0.0188(6) Uani 1 1 d . . . . .
H1 H 0.036120 0.182552 0.822538 0.023 Uiso 1 1 calc R U . . .
C2 C 0.0671(3) 0.1590(2) 0.6646(2) 0.0173(6) Uani 1 1 d . . . . .
H2A H -0.021058 0.182323 0.636945 0.021 Uiso 1 1 calc R U . . .
H2B H 0.040413 0.075270 0.633557 0.021 Uiso 1 1 calc R U . . .
C3 C 0.1898(3) 0.1994(2) 0.6212(2) 0.0140(6) Uani 1 1 d . . . . .
C4 C 0.2297(3) 0.3307(2) 0.6734(2) 0.0140(6) Uani 1 1 d . . . . .
H4A H 0.308294 0.358404 0.646244 0.017 Uiso 1 1 calc R U . . .
H4B H 0.142730 0.355203 0.645716 0.017 Uiso 1 1 calc R U . . .
C5 C 0.2819(3) 0.3847(2) 0.8061(2) 0.0151(6) Uani 1 1 d . . . . .
C6 C 0.1575(3) 0.3395(2) 0.8453(2) 0.0172(6) Uani 1 1 d . . . . .
H6A H 0.188849 0.371414 0.930119 0.021 Uiso 1 1 calc R U . . .
H6B H 0.069970 0.364390 0.819474 0.021 Uiso 1 1 calc R U . . .
C7 C 0.2515(3) 0.1717(2) 0.8395(2) 0.0204(7) Uani 1 1 d . . . . .
H7A H 0.226593 0.088093 0.809190 0.025 Uiso 1 1 calc R U . . .
H7B H 0.283379 0.203432 0.924256 0.025 Uiso 1 1 calc R U . . .
C8 C 0.3258(3) 0.1641(2) 0.6678(2) 0.0170(6) Uani 1 1 d . . . . .
H8A H 0.302767 0.080460 0.636411 0.020 Uiso 1 1 calc R U . . .
H8B H 0.406642 0.190758 0.642047 0.020 Uiso 1 1 calc R U . . .
C9 C 0.3753(3) 0.2137(2) 0.7990(2) 0.0177(6) Uani 1 1 d . . . . .
H9 H 0.463210 0.188818 0.826464 0.021 Uiso 1 1 calc R U . . .
C10 C 0.4155(3) 0.3435(2) 0.8481(2) 0.0162(6) Uani 1 1 d . . . . .
H10A H 0.497435 0.370570 0.823667 0.019 Uiso 1 1 calc R U . . .
H10B H 0.448347 0.375417 0.932916 0.019 Uiso 1 1 calc R U . . .
C11 C 0.1384(3) 0.1540(2) 0.4906(2) 0.0139(6) Uani 1 1 d . . . . .
C12 C 0.2213(3) 0.1000(2) 0.4245(2) 0.0151(6) Uani 1 1 d . . . . .
H12 H 0.309780 0.087930 0.461001 0.018 Uiso 1 1 calc R U . . .
C13 C 0.1759(3) 0.0638(2) 0.3064(2) 0.0163(6) Uani 1 1 d . . . . .
C14 C 0.0471(3) 0.0794(2) 0.2500(2) 0.0151(6) Uani 1 1 d . . . . .
C15 C -0.0365(3) 0.1326(2) 0.3150(2) 0.0150(6) Uani 1 1 d . . . . .
C16 C 0.0082(3) 0.1691(2) 0.4333(2) 0.0154(6) Uani 1 1 d . . . . .
H16 H -0.050626 0.204930 0.476001 0.018 Uiso 1 1 calc R U . . .
C17 C 0.3764(3) -0.0197(3) 0.2852(3) 0.0277(7) Uani 1 1 d . . . . .
H17A H 0.419666 -0.056918 0.225993 0.042 Uiso 1 1 calc R U . . .
H17B H 0.346629 -0.071501 0.318523 0.042 Uiso 1 1 calc R U . . .
H17C H 0.448816 0.048847 0.345378 0.042 Uiso 1 1 calc R U . . .
C18 C -0.2666(3) 0.1782(3) 0.3093(3) 0.0252(7) Uani 1 1 d . . . . .
H18A H -0.357827 0.170567 0.253159 0.038 Uiso 1 1 calc R U . . .
H18B H -0.226559 0.257351 0.365310 0.038 Uiso 1 1 calc R U . . .
H18C H -0.286600 0.130231 0.348852 0.038 Uiso 1 1 calc R U . . .
C19 C 0.3244(3) 0.5135(2) 0.8495(2) 0.0149(6) Uani 1 1 d . . . . .
C20 C 0.2542(3) 0.5823(2) 0.9162(2) 0.0180(6) Uani 1 1 d . . . . .
H20 H 0.177197 0.549017 0.936647 0.022 Uiso 1 1 calc R U . . .
C21 C 0.2954(3) 0.6988(2) 0.9530(2) 0.0185(6) Uani 1 1 d . . . . .
C22 C 0.4084(3) 0.7505(2) 0.9276(2) 0.0181(6) Uani 1 1 d . . . . .
C23 C 0.4817(3) 0.6827(2) 0.8622(2) 0.0177(6) Uani 1 1 d . . . . .
C24 C 0.4394(3) 0.5659(2) 0.8236(2) 0.0167(6) Uani 1 1 d . . . . .
H24 H 0.489560 0.520733 0.778774 0.020 Uiso 1 1 calc R U . . .
C25 C 0.0802(4) 0.7515(3) 0.9821(3) 0.0485(11) Uani 1 1 d . . . . .
H25A H 0.052614 0.744631 0.903149 0.073 Uiso 1 1 calc R U . . .
H25B H 0.050039 0.815013 1.030373 0.073 Uiso 1 1 calc R U . . .
H25C H 0.031475 0.681349 0.983553 0.073 Uiso 1 1 calc R U . . .
C26 C 0.6924(3) 0.6831(3) 0.7971(3) 0.0282(7) Uani 1 1 d . . . . .
H26A H 0.639964 0.625363 0.719129 0.042 Uiso 1 1 calc R U . . .
H26B H 0.732172 0.646664 0.845667 0.042 Uiso 1 1 calc R U . . .
H26C H 0.772874 0.736702 0.795259 0.042 Uiso 1 1 calc R U . . .
O1 O 0.2516(2) 0.00998(17) 0.23544(16) 0.0227(5) Uani 1 1 d . . . . .
O2 O 0.0090(2) 0.04156(17) 0.13354(16) 0.0216(5) Uani 1 1 d . . . . .
H2 H -0.079372 0.039599 0.107468 0.032 Uiso 1 1 calc R U . . .
O3 O -0.1627(2) 0.14368(16) 0.25174(15) 0.0187(4) Uani 1 1 d . . . . .
O4 O 0.2320(2) 0.77078(17) 1.02360(18) 0.0281(5) Uani 1 1 d . . . . .
O5 O 0.4551(2) 0.86528(15) 0.96547(17) 0.0210(5) Uani 1 1 d . . . . .
H5 H 0.386376 0.894363 0.978708 0.032 Uiso 1 1 calc R U . . .
O6 O 0.5935(2) 0.74231(16) 0.84255(17) 0.0233(5) Uani 1 1 d . . . . .
O7 O 0.2680(2) 1.00229(17) 1.01689(17) 0.0199(5) Uani 1 1 d . . . . .
H7C H 0.336(4) 1.058(3) 1.033(3) 0.030 Uiso 1 1 d . U . . .
H7D H 0.243(4) 1.012(3) 1.072(3) 0.030 Uiso 1 1 d . U . . .
C27 C 0.6752(3) 0.4036(2) 0.5470(3) 0.0228(7) Uani 1 1 d . . . . .
C28 C 0.7736(3) 0.4099(3) 0.6449(3) 0.0253(7) Uani 1 1 d . . . . .
C29 C 0.9076(3) 0.4906(3) 0.6953(3) 0.0261(7) Uani 1 1 d . . . . .
H29 H 0.975768 0.494226 0.761735 0.031 Uiso 1 1 calc R U . . .
C30 C 0.9415(4) 0.5653(3) 0.6489(3) 0.0307(8) Uani 1 1 d . . . . .
H30 H 1.032597 0.621503 0.684029 0.037 Uiso 1 1 calc R U . . .
C31 C 0.8427(4) 0.5589(3) 0.5509(3) 0.0368(9) Uani 1 1 d . . . . .
H31 H 0.866814 0.610568 0.518985 0.044 Uiso 1 1 calc R U . . .
C32 C 0.7100(4) 0.4780(3) 0.4995(3) 0.0301(8) Uani 1 1 d . . . . .
H32 H 0.642977 0.473413 0.432012 0.036 Uiso 1 1 calc R U . . .
Cl1 Cl 0.50652(8) 0.30309(7) 0.48215(7) 0.0346(2) Uani 1 1 d . . . . .
Cl2 Cl 0.73260(9) 0.31834(8) 0.70674(9) 0.0471(3) Uani 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 0.0033 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'
Cl Cl 0.1484 0.1585 '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'
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
C7 C1 C2 109.8(2) . . ?
C7 C1 C6 109.2(2) . . ?
C2 C1 C6 109.9(2) . . ?
C7 C1 H1 109.3 . . ?
C2 C1 H1 109.3 . . ?
C6 C1 H1 109.3 . . ?
C1 C2 C3 110.6(2) . . ?
C1 C2 H2A 109.5 . . ?
C3 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C11 C3 C8 113.1(2) . . ?
C11 C3 C2 111.0(2) . . ?
C8 C3 C2 108.2(2) . . ?
C11 C3 C4 108.8(2) . . ?
C8 C3 C4 107.8(2) . . ?
C2 C3 C4 107.8(2) . . ?
C5 C4 C3 112.6(2) . . ?
C5 C4 H4A 109.1 . . ?
C3 C4 H4A 109.1 . . ?
C5 C4 H4B 109.1 . . ?
C3 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
C19 C5 C6 113.7(2) . . ?
C19 C5 C10 110.5(2) . . ?
C6 C5 C10 107.5(2) . . ?
C19 C5 C4 108.9(2) . . ?
C6 C5 C4 107.7(2) . . ?
C10 C5 C4 108.5(2) . . ?
C1 C6 C5 111.0(2) . . ?
C1 C6 H6A 109.4 . . ?
C5 C6 H6A 109.4 . . ?
C1 C6 H6B 109.4 . . ?
C5 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
C1 C7 C9 108.8(2) . . ?
C1 C7 H7A 109.9 . . ?
C9 C7 H7A 109.9 . . ?
C1 C7 H7B 109.9 . . ?
C9 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
C9 C8 C3 111.2(2) . . ?
C9 C8 H8A 109.4 . . ?
C3 C8 H8A 109.4 . . ?
C9 C8 H8B 109.4 . . ?
C3 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
C7 C9 C8 109.8(2) . . ?
C7 C9 C10 109.7(2) . . ?
C8 C9 C10 109.6(2) . . ?
C7 C9 H9 109.2 . . ?
C8 C9 H9 109.2 . . ?
C10 C9 H9 109.2 . . ?
C9 C10 C5 110.5(2) . . ?
C9 C10 H10A 109.5 . . ?
C5 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C5 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
C12 C11 C16 117.7(2) . . ?
C12 C11 C3 121.6(2) . . ?
C16 C11 C3 120.6(2) . . ?
C13 C12 C11 120.8(3) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
O1 C13 C14 114.4(2) . . ?
O1 C13 C12 124.2(2) . . ?
C14 C13 C12 121.3(2) . . ?
O2 C14 C13 118.2(2) . . ?
O2 C14 C15 123.5(2) . . ?
C13 C14 C15 118.3(2) . . ?
O3 C15 C16 125.1(2) . . ?
O3 C15 C14 114.2(2) . . ?
C16 C15 C14 120.7(2) . . ?
C15 C16 C11 121.2(2) . . ?
C15 C16 H16 119.4 . . ?
C11 C16 H16 119.4 . . ?
O1 C17 H17A 109.5 . . ?
O1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O3 C18 H18A 109.5 . . ?
O3 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O3 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 C24 117.9(2) . . ?
C20 C19 C5 122.6(2) . . ?
C24 C19 C5 119.5(2) . . ?
C21 C20 C19 120.7(3) . . ?
C21 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
C22 C21 C20 121.5(3) . . ?
C22 C21 O4 116.0(2) . . ?
C20 C21 O4 122.4(3) . . ?
O5 C22 C21 123.1(3) . . ?
O5 C22 C23 118.4(2) . . ?
C21 C22 C23 118.5(2) . . ?
O6 C23 C24 125.7(3) . . ?
O6 C23 C22 114.0(2) . . ?
C24 C23 C22 120.3(3) . . ?
C23 C24 C19 121.1(3) . . ?
C23 C24 H24 119.4 . . ?
C19 C24 H24 119.4 . . ?
O4 C25 H25A 109.5 . . ?
O4 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O4 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O6 C26 H26A 109.5 . . ?
O6 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
O6 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C13 O1 C17 117.8(2) . . ?
C14 O2 H2 109.5 . . ?
C15 O3 C18 117.1(2) . . ?
C21 O4 C25 116.4(2) . . ?
C22 O5 H5 109.5 . . ?
C23 O6 C26 117.6(2) . . ?
H7C O7 H7D 108(3) . . ?
C32 C27 C28 120.2(3) . . ?
C32 C27 Cl1 118.9(2) . . ?
C28 C27 Cl1 120.9(2) . . ?
C29 C28 C27 120.0(3) . . ?
C29 C28 Cl2 118.8(2) . . ?
C27 C28 Cl2 121.2(2) . . ?
C30 C29 C28 119.8(3) . . ?
C30 C29 H29 120.1 . . ?
C28 C29 H29 120.1 . . ?
C29 C30 C31 120.1(3) . . ?
C29 C30 H30 120.0 . . ?
C31 C30 H30 120.0 . . ?
C32 C31 C30 120.5(3) . . ?
C32 C31 H31 119.8 . . ?
C30 C31 H31 119.8 . . ?
C31 C32 C27 119.4(3) . . ?
C31 C32 H32 120.3 . . ?
C27 C32 H32 120.3 . . ?
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 C7 1.528(4) . ?
C1 C2 1.536(4) . ?
C1 C6 1.537(4) . ?
C1 H1 1.0000 . ?
C2 C3 1.541(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C11 1.528(4) . ?
C3 C8 1.536(4) . ?
C3 C4 1.551(4) . ?
C4 C5 1.548(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C19 1.527(4) . ?
C5 C6 1.541(4) . ?
C5 C10 1.547(4) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C9 1.531(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.532(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.534(4) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.399(4) . ?
C11 C16 1.399(4) . ?
C12 C13 1.388(4) . ?
C12 H12 0.9500 . ?
C13 O1 1.381(3) . ?
C13 C14 1.387(4) . ?
C14 O2 1.366(3) . ?
C14 C15 1.394(4) . ?
C15 O3 1.376(3) . ?
C15 C16 1.388(4) . ?
C16 H16 0.9500 . ?
C17 O1 1.422(3) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 O3 1.428(3) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.393(4) . ?
C19 C24 1.397(4) . ?
C20 C21 1.386(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.374(4) . ?
C21 O4 1.392(3) . ?
C22 O5 1.367(3) . ?
C22 C23 1.399(4) . ?
C23 O6 1.371(3) . ?
C23 C24 1.388(4) . ?
C24 H24 0.9500 . ?
C25 O4 1.396(4) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 O6 1.428(4) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
O2 H2 0.8400 . ?
O5 H5 0.8400 . ?
O7 H7C 0.83(4) . ?
O7 H7D 0.79(4) . ?
C27 C32 1.385(4) . ?
C27 C28 1.385(4) . ?
C27 Cl1 1.738(3) . ?
C28 C29 1.385(4) . ?
C28 Cl2 1.733(3) . ?
C29 C30 1.374(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.387(5) . ?
C30 H30 0.9500 . ?
C31 C32 1.378(5) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O2 H2 O3 0.84 2.30 2.713(3) 110.7 . yes
O2 H2 O7 0.84 2.00 2.781(3) 154.6 2_566 yes
O5 H5 O7 0.84 1.96 2.773(3) 163.1 . yes
O7 H7C O5 0.83(4) 2.11(4) 2.880(3) 154(3) 2_677 yes
O7 H7C O6 0.83(4) 2.42(3) 3.070(3) 136(3) 2_677 yes
O7 H7D O1 0.79(4) 2.14(4) 2.892(3) 157(3) 1_566 yes
O7 H7D O2 0.79(4) 2.62(3) 3.250(3) 137(3) 1_566 yes
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
C7 C1 C2 C3 -60.4(3) . . . . ?
C6 C1 C2 C3 59.8(3) . . . . ?
C1 C2 C3 C11 -177.3(2) . . . . ?
C1 C2 C3 C8 58.0(3) . . . . ?
C1 C2 C3 C4 -58.3(3) . . . . ?
C11 C3 C4 C5 179.4(2) . . . . ?
C8 C3 C4 C5 -57.6(3) . . . . ?
C2 C3 C4 C5 59.0(3) . . . . ?
C3 C4 C5 C19 177.7(2) . . . . ?
C3 C4 C5 C6 -58.6(3) . . . . ?
C3 C4 C5 C10 57.4(3) . . . . ?
C7 C1 C6 C5 60.9(3) . . . . ?
C2 C1 C6 C5 -59.7(3) . . . . ?
C19 C5 C6 C1 178.5(2) . . . . ?
C10 C5 C6 C1 -58.9(3) . . . . ?
C4 C5 C6 C1 57.8(3) . . . . ?
C2 C1 C7 C9 60.3(3) . . . . ?
C6 C1 C7 C9 -60.3(3) . . . . ?
C11 C3 C8 C9 178.7(2) . . . . ?
C2 C3 C8 C9 -57.9(3) . . . . ?
C4 C3 C8 C9 58.4(3) . . . . ?
C1 C7 C9 C8 -59.8(3) . . . . ?
C1 C7 C9 C10 60.7(3) . . . . ?
C3 C8 C9 C7 59.8(3) . . . . ?
C3 C8 C9 C10 -60.7(3) . . . . ?
C7 C9 C10 C5 -60.8(3) . . . . ?
C8 C9 C10 C5 59.7(3) . . . . ?
C19 C5 C10 C9 -176.8(2) . . . . ?
C6 C5 C10 C9 58.7(3) . . . . ?
C4 C5 C10 C9 -57.5(3) . . . . ?
C8 C3 C11 C12 -8.3(4) . . . . ?
C2 C3 C11 C12 -130.2(3) . . . . ?
C4 C3 C11 C12 111.4(3) . . . . ?
C8 C3 C11 C16 174.0(2) . . . . ?
C2 C3 C11 C16 52.1(3) . . . . ?
C4 C3 C11 C16 -66.3(3) . . . . ?
C16 C11 C12 C13 0.6(4) . . . . ?
C3 C11 C12 C13 -177.2(2) . . . . ?
C11 C12 C13 O1 180.0(2) . . . . ?
C11 C12 C13 C14 -0.3(4) . . . . ?
O1 C13 C14 O2 -0.2(4) . . . . ?
C12 C13 C14 O2 -180.0(2) . . . . ?
O1 C13 C14 C15 179.8(2) . . . . ?
C12 C13 C14 C15 0.0(4) . . . . ?
O2 C14 C15 O3 0.4(4) . . . . ?
C13 C14 C15 O3 -179.6(2) . . . . ?
O2 C14 C15 C16 180.0(2) . . . . ?
C13 C14 C15 C16 0.0(4) . . . . ?
O3 C15 C16 C11 179.8(2) . . . . ?
C14 C15 C16 C11 0.3(4) . . . . ?
C12 C11 C16 C15 -0.6(4) . . . . ?
C3 C11 C16 C15 177.2(2) . . . . ?
C6 C5 C19 C20 -1.3(4) . . . . ?
C10 C5 C19 C20 -122.1(3) . . . . ?
C4 C5 C19 C20 118.8(3) . . . . ?
C6 C5 C19 C24 177.7(2) . . . . ?
C10 C5 C19 C24 56.8(3) . . . . ?
C4 C5 C19 C24 -62.3(3) . . . . ?
C24 C19 C20 C21 1.6(4) . . . . ?
C5 C19 C20 C21 -179.5(2) . . . . ?
C19 C20 C21 C22 -1.6(4) . . . . ?
C19 C20 C21 O4 -177.3(2) . . . . ?
C20 C21 C22 O5 -177.9(2) . . . . ?
O4 C21 C22 O5 -1.8(4) . . . . ?
C20 C21 C22 C23 0.5(4) . . . . ?
O4 C21 C22 C23 176.5(2) . . . . ?
O5 C22 C23 O6 -0.9(4) . . . . ?
C21 C22 C23 O6 -179.4(2) . . . . ?
O5 C22 C23 C24 179.0(2) . . . . ?
C21 C22 C23 C24 0.5(4) . . . . ?
O6 C23 C24 C19 179.4(2) . . . . ?
C22 C23 C24 C19 -0.5(4) . . . . ?
C20 C19 C24 C23 -0.5(4) . . . . ?
C5 C19 C24 C23 -179.6(2) . . . . ?
C14 C13 O1 C17 -173.5(2) . . . . ?
C12 C13 O1 C17 6.2(4) . . . . ?
C16 C15 O3 C18 -10.8(4) . . . . ?
C14 C15 O3 C18 168.8(2) . . . . ?
C22 C21 O4 C25 125.9(3) . . . . ?
C20 C21 O4 C25 -58.1(4) . . . . ?
C24 C23 O6 C26 -12.2(4) . . . . ?
C22 C23 O6 C26 167.7(2) . . . . ?
C32 C27 C28 C29 -0.3(5) . . . . ?
Cl1 C27 C28 C29 180.0(2) . . . . ?
C32 C27 C28 Cl2 179.6(2) . . . . ?
Cl1 C27 C28 Cl2 -0.1(4) . . . . ?
C27 C28 C29 C30 1.0(5) . . . . ?
Cl2 C28 C29 C30 -178.9(2) . . . . ?
C28 C29 C30 C31 -1.0(5) . . . . ?
C29 C30 C31 C32 0.2(5) . . . . ?
C30 C31 C32 C27 0.5(5) . . . . ?
C28 C27 C32 C31 -0.5(5) . . . . ?
Cl1 C27 C32 C31 179.3(3) . . . . ?
