#------------------------------------------------------------------------------
#$Date: 2022-01-01 07:12:04 +0200 (Sat, 01 Jan 2022) $
#$Revision: 271675 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/58/1565856.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_1565856
loop_
_publ_author_name
'Malinska, Maura'
_publ_section_title
;
 Insights into molecular recognition from the crystal structures of
 p-tert-butylcalix[6]arene complexed with different solvents
;
_journal_coeditor_code           ED5024
_journal_issue                   1
_journal_name_full               IUCrJ
_journal_page_first              55
_journal_page_last               64
_journal_paper_doi               10.1107/S2052252521010678
_journal_volume                  9
_journal_year                    2022
_chemical_formula_moiety         'C66 H84 O6, 2(C H2 Cl2)'
_chemical_formula_sum            'C68 H88 Cl4 O6'
_chemical_formula_weight         1143.18
_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
_atom_sites_solution_primary     direct
_cell_angle_alpha                118.625(7)
_cell_angle_beta                 92.647(5)
_cell_angle_gamma                98.062(5)
_cell_formula_units_Z            2
_cell_length_a                   12.2610(7)
_cell_length_b                   17.2425(11)
_cell_length_c                   17.4170(12)
_cell_measurement_reflns_used    13662
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      71.4760
_cell_measurement_theta_min      5.6660
_cell_volume                     3172.8(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37155
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.724
_diffrn_reflns_theta_min         2.915
_exptl_absorpt_coefficient_mu    2.077
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50578
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         12208
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0508
_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)+(0.0679P)²+2.1130P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1299
_refine_ls_wR_factor_ref         0.1415
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9900
_reflns_number_total             12208
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ed5024.cif
_cod_data_source_block           13_x6_DCM_1_2
_cod_database_code               1565856
_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   0.819
_shelx_estimated_absorpt_t_min   0.575
_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, All O(H) groups
2. Restrained distances
 Cl1A-C67
 1.81 with sigma of 0.02
 C67-Cl2
 1.81 with sigma of 0.02
 C67A-Cl2A
 1.81 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C8) = Uanis(C8A)
Uanis(C10) = Uanis(C10A)
Uanis(C9A) = Uanis(C9)
Uanis(C68) = Uanis(C68A)
Uanis(Cl4A) = Uanis(Cl4)
Uanis(Cl1A) = Uanis(Cl1)
Uanis(C67A) = Uanis(C67)
Uanis(Cl2A) = Uanis(Cl2)
4. Others
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=
 Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(1)
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(1)
 Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(Cl4A)=Sof(Cl3A)=1-FVAR(2)
 Sof(C68A)=Sof(H68C)=Sof(H68D)=Sof(Cl4)=Sof(Cl3)=FVAR(2)
 Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(Cl1A)=Sof(Cl2)=1-FVAR(3)
 Sof(C67A)=Sof(H67C)=Sof(H67D)=Sof(Cl1)=Sof(Cl2A)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C22(H22A,H22B), C33(H33A,H33B), C44(H44A,H44B), C55(H55A,
 H55B), C66(H66A,H66B), C67(H67A,H67B), C67A(H67C,H67D), C68(H68A,H68B),
 C68A(H68C,H68D)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C13(H13), C15(H15), C24(H24), C26(H26), C35(H35), C37(H37),
 C48(H48), C50(H50), C57(H57), C59(H59)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C8A(H8AA,H8AB,H8AC), C9(H9A,H9B,H9C), C9A(H9AA,H9AB,H9AC),
 C10(H10A,H10B,H10C), C10A(H10D,H10E,H10F), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C),
 C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C63(H63A,H63B,
 H63C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C)
5.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O3(H3A), O4(H4), O5(H5A), O6(H6)
;
_olex2_submission_special_instructions 'No special instructions were received'
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 0.75091(15) 0.14472(12) 0.13762(12) 0.0160(4) Uani 1 1 d . . . . .
C2 C 0.65335(16) 0.17232(12) 0.16999(12) 0.0167(4) Uani 1 1 d . . . . .
C3 C 0.56991(16) 0.10936(12) 0.17142(12) 0.0183(4) Uani 1 1 d . . . . .
H3 H 0.5033 0.1279 0.1936 0.022 Uiso 1 1 calc R . . . .
C4 C 0.58021(16) 0.02018(12) 0.14158(12) 0.0179(4) Uani 1 1 d . . . . .
C5 C 0.67793(16) -0.00481(12) 0.10725(12) 0.0172(4) Uani 1 1 d . . . . .
H5 H 0.6862 -0.0656 0.0847 0.021 Uiso 1 1 calc R . . . .
C6 C 0.76343(15) 0.05516(12) 0.10456(12) 0.0161(4) Uani 1 1 d . . . . .
C7 C 0.48910(17) -0.04849(13) 0.14424(14) 0.0222(4) Uani 1 1 d . . . . .
C8 C 0.3967(3) -0.00707(19) 0.1955(2) 0.0364(7) Uani 0.808(3) 1 d . . P A 1
H8A H 0.4280 0.0379 0.2562 0.055 Uiso 0.808(3) 1 calc GR . P A 1
H8B H 0.3422 -0.0541 0.1959 0.055 Uiso 0.808(3) 1 calc GR . P A 1
H8C H 0.3603 0.0217 0.1674 0.055 Uiso 0.808(3) 1 calc GR . P A 1
C8A C 0.4547(11) -0.0050(8) 0.2371(10) 0.0364(7) Uani 0.192(3) 1 d . . P A 2
H8AA H 0.5176 0.0062 0.2801 0.055 Uiso 0.192(3) 1 calc GR . P A 2
H8AB H 0.3924 -0.0455 0.2399 0.055 Uiso 0.192(3) 1 calc GR . P A 2
H8AC H 0.4321 0.0520 0.2505 0.055 Uiso 0.192(3) 1 calc GR . P A 2
C9 C 0.5402(2) -0.0976(2) 0.1879(2) 0.0381(7) Uani 0.808(3) 1 d . . P A 1
H9A H 0.5969 -0.1284 0.1537 0.057 Uiso 0.808(3) 1 calc GR . P A 1
H9B H 0.4817 -0.1418 0.1893 0.057 Uiso 0.808(3) 1 calc GR . P A 1
H9C H 0.5741 -0.0537 0.2482 0.057 Uiso 0.808(3) 1 calc GR . P A 1
C9A C 0.5191(11) -0.1341(9) 0.1185(11) 0.0381(7) Uani 0.192(3) 1 d . . P A 2
H9AA H 0.5269 -0.1640 0.0555 0.057 Uiso 0.192(3) 1 calc GR . P A 2
H9AB H 0.4611 -0.1714 0.1297 0.057 Uiso 0.192(3) 1 calc GR . P A 2
H9AC H 0.5898 -0.1256 0.1527 0.057 Uiso 0.192(3) 1 calc GR . P A 2
C10 C 0.4393(3) -0.1193(2) 0.0492(2) 0.0421(8) Uani 0.808(3) 1 d . . P A 1
H10A H 0.4091 -0.0897 0.0193 0.063 Uiso 0.808(3) 1 calc GR . P A 1
H10B H 0.3797 -0.1629 0.0504 0.063 Uiso 0.808(3) 1 calc GR . P A 1
H10C H 0.4973 -0.1505 0.0175 0.063 Uiso 0.808(3) 1 calc GR . P A 1
C10A C 0.3861(12) -0.0598(9) 0.0794(9) 0.0421(8) Uani 0.192(3) 1 d . . P A 2
H10D H 0.3600 -0.0026 0.1017 0.063 Uiso 0.192(3) 1 calc GR . P A 2
H10E H 0.3263 -0.1061 0.0755 0.063 Uiso 0.192(3) 1 calc GR . P A 2
H10F H 0.4083 -0.0777 0.0207 0.063 Uiso 0.192(3) 1 calc GR . P A 2
C11 C 0.86812(15) 0.02382(12) 0.06760(12) 0.0167(4) Uani 1 1 d . . . . .
H11A H 0.8770 -0.0291 0.0739 0.020 Uiso 1 1 calc R . . . .
H11B H 0.9327 0.0721 0.1033 0.020 Uiso 1 1 calc R . . . .
C12 C 0.86973(15) -0.00104(12) -0.02846(12) 0.0162(4) Uani 1 1 d . . . . .
C13 C 0.82978(15) -0.08898(12) -0.09494(13) 0.0176(4) Uani 1 1 d . . . . .
H13 H 0.7995 -0.1321 -0.0788 0.021 Uiso 1 1 calc R . . . .
C14 C 0.83223(15) -0.11648(12) -0.18417(12) 0.0179(4) Uani 1 1 d . . . . .
C15 C 0.87372(16) -0.05161(12) -0.20654(12) 0.0180(4) Uani 1 1 d . . . . .
H15 H 0.8748 -0.0685 -0.2670 0.022 Uiso 1 1 calc R . . . .
C16 C 0.91390(15) 0.03781(12) -0.14227(12) 0.0167(4) Uani 1 1 d . . . . .
C17 C 0.91331(15) 0.06095(12) -0.05414(12) 0.0163(4) Uani 1 1 d . . . . .
C18 C 0.79229(16) -0.21636(12) -0.25223(12) 0.0188(4) Uani 1 1 d . . . . .
C19 C 0.86711(17) -0.27229(13) -0.23454(13) 0.0231(4) Uani 1 1 d . . . . .
H19A H 0.9436 -0.2549 -0.2423 0.035 Uiso 1 1 calc GR . . . .
H19B H 0.8404 -0.3363 -0.2761 0.035 Uiso 1 1 calc GR . . . .
H19C H 0.8649 -0.2613 -0.1740 0.035 Uiso 1 1 calc GR . . . .
C20 C 0.79690(19) -0.23452(13) -0.34678(13) 0.0265(4) Uani 1 1 d . . . . .
H20A H 0.7516 -0.1978 -0.3583 0.040 Uiso 1 1 calc GR . . . .
H20B H 0.7680 -0.2983 -0.3880 0.040 Uiso 1 1 calc GR . . . .
H20C H 0.8740 -0.2192 -0.3548 0.040 Uiso 1 1 calc GR . . . .
C21 C 0.67134(17) -0.24494(13) -0.24331(14) 0.0243(4) Uani 1 1 d . . . . .
H21A H 0.6659 -0.2321 -0.1825 0.037 Uiso 1 1 calc GR . . . .
H21B H 0.6470 -0.3095 -0.2837 0.037 Uiso 1 1 calc GR . . . .
H21C H 0.6239 -0.2115 -0.2581 0.037 Uiso 1 1 calc GR . . . .
C22 C 0.95982(16) 0.10639(12) -0.16987(12) 0.0178(4) Uani 1 1 d . . . . .
H22A H 0.9922 0.0752 -0.2254 0.021 Uiso 1 1 calc R . . . .
H22B H 1.0204 0.1513 -0.1240 0.021 Uiso 1 1 calc R . . . .
C23 C 0.87276(15) 0.15546(12) -0.18359(12) 0.0170(4) Uani 1 1 d . . . . .
C24 C 0.82597(16) 0.13045(12) -0.26810(12) 0.0178(4) Uani 1 1 d . . . . .
H24 H 0.8510 0.0838 -0.3169 0.021 Uiso 1 1 calc R . . . .
C25 C 0.74325(16) 0.17115(12) -0.28438(12) 0.0186(4) Uani 1 1 d . . . . .
C26 C 0.70867(16) 0.23968(12) -0.21160(12) 0.0177(4) Uani 1 1 d . . . . .
H26 H 0.6529 0.2686 -0.2208 0.021 Uiso 1 1 calc R . . . .
C27 C 0.75357(16) 0.26719(11) -0.12540(12) 0.0170(4) Uani 1 1 d . . . . .
C28 C 0.83584(16) 0.22517(12) -0.11271(12) 0.0177(4) Uani 1 1 d . . . . .
C29 C 0.69374(18) 0.13839(14) -0.37957(13) 0.0258(4) Uani 1 1 d . . . . .
C30 C 0.7861(2) 0.1534(2) -0.42996(17) 0.0477(7) Uani 1 1 d . . . . .
H30A H 0.7549 0.1333 -0.4907 0.072 Uiso 1 1 calc GR . . . .
H30B H 0.8434 0.1189 -0.4305 0.072 Uiso 1 1 calc GR . . . .
H30C H 0.8190 0.2174 -0.4009 0.072 Uiso 1 1 calc GR . . . .
C31 C 0.6006(2) 0.18705(15) -0.38436(15) 0.0328(5) Uani 1 1 d . . . . .
H31A H 0.5704 0.1630 -0.4462 0.049 Uiso 1 1 calc GR . . . .
H31B H 0.6302 0.2515 -0.3580 0.049 Uiso 1 1 calc GR . . . .
H31C H 0.5415 0.1778 -0.3520 0.049 Uiso 1 1 calc GR . . . .
C32 C 0.6440(2) 0.03729(15) -0.42337(16) 0.0397(6) Uani 1 1 d . . . . .
H32A H 0.5835 0.0281 -0.3920 0.060 Uiso 1 1 calc GR . . . .
H32B H 0.7018 0.0044 -0.4208 0.060 Uiso 1 1 calc GR . . . .
H32C H 0.6151 0.0151 -0.4851 0.060 Uiso 1 1 calc GR . . . .
C33 C 0.70958(16) 0.33864(12) -0.04695(12) 0.0185(4) Uani 1 1 d . . . . .
H33A H 0.7155 0.3249 0.0020 0.022 Uiso 1 1 calc R . . . .
H33B H 0.6297 0.3339 -0.0637 0.022 Uiso 1 1 calc R . . . .
C34 C 0.76726(16) 0.43558(12) -0.01258(12) 0.0168(4) Uani 1 1 d . . . . .
C35 C 0.72041(16) 0.48910(12) -0.03974(12) 0.0189(4) Uani 1 1 d . . . . .
H35 H 0.6561 0.4625 -0.0824 0.023 Uiso 1 1 calc R . . . .
C36 C 0.76377(16) 0.57989(12) -0.00711(12) 0.0185(4) Uani 1 1 d . . . . .
C37 C 0.85722(16) 0.61745(12) 0.05662(12) 0.0183(4) Uani 1 1 d . . . . .
H37 H 0.8878 0.6794 0.0807 0.022 Uiso 1 1 calc R . . . .
C38 C 0.90737(16) 0.56676(12) 0.08629(12) 0.0175(4) Uani 1 1 d . . . . .
C39 C 0.86295(16) 0.47564(12) 0.04920(12) 0.0169(4) Uani 1 1 d . . . . .
C40 C 0.70643(17) 0.63270(13) -0.04160(13) 0.0218(4) Uani 1 1 d . . . . .
C41 C 0.7047(2) 0.58798(14) -0.14192(14) 0.0296(5) Uani 1 1 d . . . . .
H41A H 0.7810 0.5870 -0.1563 0.044 Uiso 1 1 calc GR . . . .
H41B H 0.6690 0.6220 -0.1642 0.044 Uiso 1 1 calc GR . . . .
H41C H 0.6629 0.5263 -0.1694 0.044 Uiso 1 1 calc GR . . . .
C42 C 0.76586(19) 0.73078(13) -0.00021(15) 0.0284(5) Uani 1 1 d . . . . .
H42A H 0.7664 0.7604 0.0639 0.043 Uiso 1 1 calc GR . . . .
H42B H 0.7267 0.7620 -0.0240 0.043 Uiso 1 1 calc GR . . . .
H42C H 0.8424 0.7327 -0.0140 0.043 Uiso 1 1 calc GR . . . .
C43 C 0.58627(18) 0.63276(14) -0.01903(16) 0.0291(5) Uani 1 1 d . . . . .
H43A H 0.5460 0.5707 -0.0453 0.044 Uiso 1 1 calc GR . . . .
H43B H 0.5490 0.6651 -0.0426 0.044 Uiso 1 1 calc GR . . . .
H43C H 0.5874 0.6626 0.0452 0.044 Uiso 1 1 calc GR . . . .
C44 C 1.00480(16) 0.60987(12) 0.15940(12) 0.0184(4) Uani 1 1 d . . . . .
H44A H 1.0419 0.6668 0.1634 0.022 Uiso 1 1 calc R . . . .
H44B H 1.0594 0.5693 0.1448 0.022 Uiso 1 1 calc R . . . .
C45 C 0.96828(15) 0.62926(12) 0.24828(12) 0.0174(4) Uani 1 1 d . . . . .
C46 C 0.97420(15) 0.57253(12) 0.28377(12) 0.0178(4) Uani 1 1 d . . . . .
C47 C 0.93627(16) 0.59117(12) 0.36452(12) 0.0180(4) Uani 1 1 d . . . . .
C48 C 0.89163(16) 0.66859(12) 0.40877(13) 0.0200(4) Uani 1 1 d . . . . .
H48 H 0.8660 0.6821 0.4637 0.024 Uiso 1 1 calc R . . . .
C49 C 0.88299(17) 0.72742(12) 0.37571(13) 0.0201(4) Uani 1 1 d . . . . .
C50 C 0.92322(16) 0.70638(12) 0.29579(12) 0.0191(4) Uani 1 1 d . . . . .
H50 H 0.9199 0.7461 0.2727 0.023 Uiso 1 1 calc R . . . .
C51 C 0.83242(18) 0.81193(13) 0.42743(13) 0.0241(4) Uani 1 1 d . . . . .
C52 C 0.71610(18) 0.78436(14) 0.44542(14) 0.0282(5) Uani 1 1 d . . . . .
H52A H 0.6687 0.7441 0.3893 0.042 Uiso 1 1 calc GR . . . .
H52B H 0.6839 0.8381 0.4788 0.042 Uiso 1 1 calc GR . . . .
H52C H 0.7214 0.7533 0.4797 0.042 Uiso 1 1 calc GR . . . .
C53 C 0.8218(2) 0.86306(15) 0.37635(16) 0.0364(6) Uani 1 1 d . . . . .
H53A H 0.7758 0.8231 0.3194 0.055 Uiso 1 1 calc GR . . . .
H53B H 0.8958 0.8836 0.3664 0.055 Uiso 1 1 calc GR . . . .
H53C H 0.7871 0.9151 0.4106 0.055 Uiso 1 1 calc GR . . . .
C54 C 0.90740(19) 0.87492(13) 0.51503(14) 0.0289(5) Uani 1 1 d . . . . .
H54A H 0.8739 0.9276 0.5498 0.043 Uiso 1 1 calc GR . . . .
H54B H 0.9806 0.8944 0.5031 0.043 Uiso 1 1 calc GR . . . .
H54C H 0.9156 0.8430 0.5481 0.043 Uiso 1 1 calc GR . . . .
C55 C 0.94487(16) 0.52924(12) 0.40343(13) 0.0199(4) Uani 1 1 d . . . . .
H55A H 1.0033 0.4939 0.3771 0.024 Uiso 1 1 calc R . . . .
H55B H 0.9696 0.5670 0.4676 0.024 Uiso 1 1 calc R . . . .
C56 C 0.83872(16) 0.46407(12) 0.39020(12) 0.0178(4) Uani 1 1 d . . . . .
C57 C 0.78748(16) 0.46938(12) 0.46178(12) 0.0189(4) Uani 1 1 d . . . . .
H57 H 0.8189 0.5159 0.5193 0.023 Uiso 1 1 calc R . . . .
C58 C 0.69183(16) 0.40934(12) 0.45305(12) 0.0190(4) Uani 1 1 d . . . . .
C59 C 0.64425(16) 0.34501(12) 0.36750(13) 0.0180(4) Uani 1 1 d . . . . .
H59 H 0.5772 0.3053 0.3594 0.022 Uiso 1 1 calc R . . . .
C60 C 0.69199(16) 0.33713(12) 0.29351(12) 0.0176(4) Uani 1 1 d . . . . .
C61 C 0.79112(16) 0.39443(12) 0.30612(12) 0.0178(4) Uani 1 1 d . . . . .
C62 C 0.64513(17) 0.41415(13) 0.53508(13) 0.0226(4) Uani 1 1 d . . . . .
C63 C 0.6184(2) 0.50772(14) 0.59359(14) 0.0314(5) Uani 1 1 d . . . . .
H63A H 0.5954 0.5118 0.6484 0.047 Uiso 1 1 calc GR . . . .
H63B H 0.5581 0.5176 0.5623 0.047 Uiso 1 1 calc GR . . . .
H63C H 0.6846 0.5535 0.6076 0.047 Uiso 1 1 calc GR . . . .
C64 C 0.7332(2) 0.39712(17) 0.58791(16) 0.0353(5) Uani 1 1 d . . . . .
H64A H 0.7527 0.3383 0.5506 0.053 Uiso 1 1 calc GR . . . .
H64B H 0.7034 0.3982 0.6396 0.053 Uiso 1 1 calc GR . . . .
H64C H 0.7996 0.4441 0.6072 0.053 Uiso 1 1 calc GR . . . .
C65 C 0.53915(19) 0.34442(15) 0.51213(15) 0.0311(5) Uani 1 1 d . . . . .
H65A H 0.5550 0.2839 0.4762 0.047 Uiso 1 1 calc GR . . . .
H65B H 0.4816 0.3548 0.4790 0.047 Uiso 1 1 calc GR . . . .
H65C H 0.5131 0.3500 0.5666 0.047 Uiso 1 1 calc GR . . . .
C66 C 0.63539(16) 0.26792(12) 0.20126(12) 0.0176(4) Uani 1 1 d . . . . .
H66A H 0.6627 0.2869 0.1591 0.021 Uiso 1 1 calc R . . . .
H66B H 0.5546 0.2679 0.1996 0.021 Uiso 1 1 calc R . . . .
O1 O 0.83904(11) 0.20310(9) 0.13661(9) 0.0219(3) Uani 1 1 d . . . . .
H1 H 0.8260 0.2557 0.1624 0.033 Uiso 1 1 calc GR . . . .
O2 O 0.96399(11) 0.14757(8) 0.00945(8) 0.0179(3) Uani 1 1 d . . . . .
H2 H 0.9341 0.1627 0.0558 0.027 Uiso 1 1 calc GR . . . .
O3 O 0.87990(13) 0.25589(9) -0.02702(9) 0.0266(3) Uani 1 1 d . . . . .
H3A H 0.9098 0.2162 -0.0241 0.040 Uiso 1 1 calc GR . . . .
O4 O 0.91485(12) 0.42775(9) 0.07931(9) 0.0218(3) Uani 1 1 d . . . . .
H4 H 0.8939 0.3725 0.0445 0.033 Uiso 1 1 calc GR . . . .
O5 O 1.01764(11) 0.49453(8) 0.24000(9) 0.0193(3) Uani 1 1 d . . . . .
H5A H 1.0092 0.4763 0.1855 0.029 Uiso 1 1 calc GR . . . .
O6 O 0.84029(12) 0.37907(9) 0.23133(9) 0.0229(3) Uani 1 1 d . . . . .
H6 H 0.8956 0.4200 0.2447 0.034 Uiso 1 1 calc GR . . . .
C67 C 0.667(2) 0.5410(18) 0.1964(19) 0.0402(7) Uani 0.113(2) 1 d D . P B 2
H67A H 0.6677 0.4895 0.1370 0.048 Uiso 0.113(2) 1 calc R . P B 2
H67B H 0.7453 0.5702 0.2220 0.048 Uiso 0.113(2) 1 calc R . P B 2
Cl1A Cl 0.5980(7) 0.6180(4) 0.1856(5) 0.0443(2) Uani 0.113(2) 1 d D . P B 2
Cl2 Cl 0.607(2) 0.5009(16) 0.2624(14) 0.0755(6) Uani 0.113(2) 1 d D . P B 2
C67A C 0.6526(3) 0.5705(2) 0.1955(2) 0.0402(7) Uani 0.887(2) 1 d D . P B 1
H67C H 0.6579 0.5337 0.1318 0.048 Uiso 0.887(2) 1 calc R . P B 1
H67D H 0.7260 0.6094 0.2248 0.048 Uiso 0.887(2) 1 calc R . P B 1
Cl1 Cl 0.55233(8) 0.63788(5) 0.20934(6) 0.0443(2) Uani 0.887(2) 1 d . . P B 1
Cl2A Cl 0.6190(2) 0.49984(17) 0.23997(14) 0.0755(6) Uani 0.887(2) 1 d D . P B 1
C68 C 0.8465(8) 0.1389(6) 0.3127(6) 0.0359(7) Uani 0.285(5) 1 d . . P C 2
H68A H 0.8614 0.1231 0.2520 0.043 Uiso 0.285(5) 1 calc R . P C 2
H68B H 0.7664 0.1419 0.3121 0.043 Uiso 0.285(5) 1 calc R . P C 2
Cl4A Cl 0.8458(12) 0.0483(9) 0.3108(7) 0.0483(5) Uani 0.285(5) 1 d . . P C 2
Cl3A Cl 0.8963(3) 0.2335(3) 0.3607(2) 0.0387(8) Uani 0.285(5) 1 d . . P C 2
C68A C 0.7860(3) 0.1449(2) 0.3419(2) 0.0359(7) Uani 0.715(5) 1 d . . P C 1
H68C H 0.7609 0.1387 0.2841 0.043 Uiso 0.715(5) 1 calc R . P C 1
H68D H 0.7217 0.1524 0.3756 0.043 Uiso 0.715(5) 1 calc R . P C 1
Cl4 Cl 0.8353(4) 0.0443(3) 0.3250(2) 0.0483(5) Uani 0.715(5) 1 d . . P C 1
Cl3 Cl 0.89034(14) 0.23948(11) 0.3993(2) 0.0720(7) Uani 0.715(5) 1 d . . P C 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
C2 C1 C6 120.82(17) . . ?
O1 C1 C2 122.28(16) . . ?
O1 C1 C6 116.90(16) . . ?
C1 C2 C3 118.39(16) . . ?
C1 C2 C66 121.66(16) . . ?
C3 C2 C66 119.93(17) . . ?
C2 C3 H3 118.7 . . ?
C2 C3 C4 122.66(17) . . ?
C4 C3 H3 118.7 . . ?
C3 C4 C7 122.56(17) . . ?
C5 C4 C3 116.76(17) . . ?
C5 C4 C7 120.68(16) . . ?
C4 C5 H5 118.6 . . ?
C6 C5 C4 122.82(17) . . ?
C6 C5 H5 118.6 . . ?
C1 C6 C11 121.41(16) . . ?
C5 C6 C1 118.50(17) . . ?
C5 C6 C11 120.09(16) . . ?
C4 C7 C8A 107.2(5) . . ?
C4 C7 C9 109.65(18) . . ?
C4 C7 C10 108.95(18) . . ?
C4 C7 C10A 105.8(5) . . ?
C8 C7 C4 113.47(17) . . ?
C8 C7 C9 107.8(2) . . ?
C8 C7 C10 109.1(2) . . ?
C8A C7 C10A 106.6(8) . . ?
C9A C7 C4 114.3(5) . . ?
C9A C7 C8A 112.6(8) . . ?
C9A C7 C10A 109.9(8) . . ?
C10 C7 C9 107.8(2) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C8A H8AA 109.5 . . ?
C7 C8A H8AB 109.5 . . ?
C7 C8A H8AC 109.5 . . ?
H8AA C8A H8AB 109.5 . . ?
H8AA C8A H8AC 109.5 . . ?
H8AB C8A H8AC 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C9A H9AA 109.5 . . ?
C7 C9A H9AB 109.5 . . ?
C7 C9A H9AC 109.5 . . ?
H9AA C9A H9AB 109.5 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C10A H10D 109.5 . . ?
C7 C10A H10E 109.5 . . ?
C7 C10A H10F 109.5 . . ?
H10D C10A H10E 109.5 . . ?
H10D C10A H10F 109.5 . . ?
H10E C10A H10F 109.5 . . ?
C6 C11 H11A 108.7 . . ?
C6 C11 H11B 108.7 . . ?
C6 C11 C12 114.35(15) . . ?
H11A C11 H11B 107.6 . . ?
C12 C11 H11A 108.7 . . ?
C12 C11 H11B 108.7 . . ?
C13 C12 C11 120.21(16) . . ?
C13 C12 C17 117.31(17) . . ?
C17 C12 C11 122.46(16) . . ?
C12 C13 H13 118.6 . . ?
C12 C13 C14 122.83(17) . . ?
C14 C13 H13 118.6 . . ?
C13 C14 C18 118.83(16) . . ?
C15 C14 C13 117.66(17) . . ?
C15 C14 C18 123.49(17) . . ?
C14 C15 H15 119.2 . . ?
C14 C15 C16 121.69(18) . . ?
C16 C15 H15 119.2 . . ?
C15 C16 C22 119.84(17) . . ?
C17 C16 C15 118.31(17) . . ?
C17 C16 C22 121.83(16) . . ?
C16 C17 C12 122.13(17) . . ?
C16 C17 O2 117.90(16) . . ?
O2 C17 C12 119.86(16) . . ?
C14 C18 C19 108.85(15) . . ?
C20 C18 C14 112.14(16) . . ?
C20 C18 C19 108.62(16) . . ?
C20 C18 C21 108.02(17) . . ?
C21 C18 C14 109.03(15) . . ?
C21 C18 C19 110.17(16) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C16 C22 H22A 108.8 . . ?
C16 C22 H22B 108.8 . . ?
C16 C22 C23 113.70(15) . . ?
H22A C22 H22B 107.7 . . ?
C23 C22 H22A 108.8 . . ?
C23 C22 H22B 108.8 . . ?
C24 C23 C22 120.33(16) . . ?
C24 C23 C28 117.69(17) . . ?
C28 C23 C22 121.97(17) . . ?
C23 C24 H24 118.6 . . ?
C23 C24 C25 122.71(17) . . ?
C25 C24 H24 118.6 . . ?
C24 C25 C29 119.67(17) . . ?
C26 C25 C24 117.39(17) . . ?
C26 C25 C29 122.93(17) . . ?
C25 C26 H26 119.1 . . ?
C25 C26 C27 121.87(17) . . ?
C27 C26 H26 119.1 . . ?
C26 C27 C33 120.71(17) . . ?
C28 C27 C26 118.58(17) . . ?
C28 C27 C33 120.66(17) . . ?
C27 C28 C23 121.75(17) . . ?
O3 C28 C23 121.53(17) . . ?
O3 C28 C27 116.72(16) . . ?
C25 C29 C32 108.86(17) . . ?
C30 C29 C25 108.97(18) . . ?
C30 C29 C32 109.7(2) . . ?
C31 C29 C25 112.36(17) . . ?
C31 C29 C30 109.29(19) . . ?
C31 C29 C32 107.65(18) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C27 C33 H33A 108.2 . . ?
C27 C33 H33B 108.2 . . ?
C27 C33 C34 116.15(15) . . ?
H33A C33 H33B 107.4 . . ?
C34 C33 H33A 108.2 . . ?
C34 C33 H33B 108.2 . . ?
C35 C34 C33 119.33(17) . . ?
C35 C34 C39 117.69(17) . . ?
C39 C34 C33 122.89(16) . . ?
C34 C35 H35 118.5 . . ?
C36 C35 C34 122.95(18) . . ?
C36 C35 H35 118.5 . . ?
C35 C36 C37 117.15(17) . . ?
C35 C36 C40 118.90(17) . . ?
C37 C36 C40 123.94(17) . . ?
C36 C37 H37 118.9 . . ?
C36 C37 C38 122.19(17) . . ?
C38 C37 H37 118.9 . . ?
C37 C38 C44 121.44(16) . . ?
C39 C38 C37 118.24(17) . . ?
C39 C38 C44 120.27(17) . . ?
C38 C39 C34 121.69(17) . . ?
O4 C39 C34 121.55(16) . . ?
O4 C39 C38 116.69(17) . . ?
C36 C40 C41 109.20(16) . . ?
C36 C40 C43 109.51(16) . . ?
C41 C40 C43 109.46(18) . . ?
C42 C40 C36 112.11(16) . . ?
C42 C40 C41 108.73(17) . . ?
C42 C40 C43 107.79(17) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C40 C43 H43A 109.5 . . ?
C40 C43 H43B 109.5 . . ?
C40 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C38 C44 H44A 109.2 . . ?
C38 C44 H44B 109.2 . . ?
C38 C44 C45 111.87(15) . . ?
H44A C44 H44B 107.9 . . ?
C45 C44 H44A 109.2 . . ?
C45 C44 H44B 109.2 . . ?
C46 C45 C44 123.37(16) . . ?
C46 C45 C50 117.93(17) . . ?
C50 C45 C44 118.66(16) . . ?
C45 C46 C47 121.71(17) . . ?
O5 C46 C45 121.06(17) . . ?
O5 C46 C47 117.23(16) . . ?
C46 C47 C55 121.22(16) . . ?
C48 C47 C46 117.93(17) . . ?
C48 C47 C55 120.85(17) . . ?
C47 C48 H48 118.7 . . ?
C47 C48 C49 122.64(18) . . ?
C49 C48 H48 118.7 . . ?
C48 C49 C51 120.35(17) . . ?
C50 C49 C48 117.12(17) . . ?
C50 C49 C51 122.53(17) . . ?
C45 C50 H50 118.7 . . ?
C49 C50 C45 122.66(17) . . ?
C49 C50 H50 118.7 . . ?
C52 C51 C49 109.27(16) . . ?
C52 C51 C53 108.23(19) . . ?
C52 C51 C54 109.85(17) . . ?
C53 C51 C49 112.07(17) . . ?
C54 C51 C49 108.91(17) . . ?
C54 C51 C53 108.50(18) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C47 C55 H55A 108.3 . . ?
C47 C55 H55B 108.3 . . ?
H55A C55 H55B 107.4 . . ?
C56 C55 C47 115.93(16) . . ?
C56 C55 H55A 108.3 . . ?
C56 C55 H55B 108.3 . . ?
C57 C56 C55 121.07(17) . . ?
C57 C56 C61 117.29(17) . . ?
C61 C56 C55 121.59(17) . . ?
C56 C57 H57 118.5 . . ?
C56 C57 C58 123.09(17) . . ?
C58 C57 H57 118.5 . . ?
C57 C58 C62 120.40(17) . . ?
C59 C58 C57 117.01(17) . . ?
C59 C58 C62 122.58(17) . . ?
C58 C59 H59 119.0 . . ?
C58 C59 C60 122.07(18) . . ?
C60 C59 H59 119.0 . . ?
C59 C60 C66 120.33(17) . . ?
C61 C60 C59 118.56(17) . . ?
C61 C60 C66 121.10(17) . . ?
C60 C61 C56 121.69(17) . . ?
O6 C61 C56 121.83(17) . . ?
O6 C61 C60 116.48(16) . . ?
C58 C62 C63 110.27(16) . . ?
C58 C62 C64 108.69(17) . . ?
C63 C62 C64 108.63(18) . . ?
C65 C62 C58 112.68(17) . . ?
C65 C62 C63 108.14(18) . . ?
C65 C62 C64 108.35(18) . . ?
C62 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
C62 C63 H63C 109.5 . . ?
H63A C63 H63B 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C62 C64 H64A 109.5 . . ?
C62 C64 H64B 109.5 . . ?
C62 C64 H64C 109.5 . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C62 C65 H65A 109.5 . . ?
C62 C65 H65B 109.5 . . ?
C62 C65 H65C 109.5 . . ?
H65A C65 H65B 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C2 C66 H66A 108.5 . . ?
C2 C66 H66B 108.5 . . ?
C60 C66 C2 115.17(15) . . ?
C60 C66 H66A 108.5 . . ?
C60 C66 H66B 108.5 . . ?
H66A C66 H66B 107.5 . . ?
C1 O1 H1 109.5 . . ?
C17 O2 H2 109.5 . . ?
C28 O3 H3A 109.5 . . ?
C39 O4 H4 109.5 . . ?
C46 O5 H5A 109.5 . . ?
C61 O6 H6 109.5 . . ?
H67A C67 H67B 107.7 . . ?
Cl1A C67 H67A 108.9 . . ?
Cl1A C67 H67B 108.9 . . ?
Cl2 C67 H67A 108.9 . . ?
Cl2 C67 H67B 108.9 . . ?
Cl2 C67 Cl1A 113.5(14) . . ?
H67C C67A H67D 108.0 . . ?
Cl1 C67A H67C 109.4 . . ?
Cl1 C67A H67D 109.4 . . ?
Cl2A C67A H67C 109.4 . . ?
Cl2A C67A H67D 109.4 . . ?
Cl2A C67A Cl1 111.16(19) . . ?
H68A C68 H68B 104.5 . . ?
Cl4A C68 H68A 101.2 . . ?
Cl4A C68 H68B 101.2 . . ?
Cl3A C68 H68A 101.2 . . ?
Cl3A C68 H68B 101.2 . . ?
Cl3A C68 Cl4A 143.2(8) . . ?
H68C C68A H68D 108.0 . . ?
Cl4 C68A H68C 109.4 . . ?
Cl4 C68A H68D 109.4 . . ?
Cl3 C68A H68C 109.4 . . ?
Cl3 C68A H68D 109.4 . . ?
Cl3 C68A Cl4 111.0(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 C2 1.393(3) . ?
C1 C6 1.401(2) . ?
C1 O1 1.376(2) . ?
C2 C3 1.394(3) . ?
C2 C66 1.522(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.395(3) . ?
C4 C5 1.394(3) . ?
C4 C7 1.529(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.385(3) . ?
C6 C11 1.514(2) . ?
C7 C8 1.516(3) . ?
C7 C8A 1.531(14) . ?
C7 C9 1.552(3) . ?
C7 C9A 1.432(13) . ?
C7 C10 1.537(3) . ?
C7 C10A 1.580(14) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8A H8AA 0.9800 . ?
C8A H8AB 0.9800 . ?
C8A H8AC 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C9A H9AA 0.9800 . ?
C9A H9AB 0.9800 . ?
C9A H9AC 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C10A H10D 0.9800 . ?
C10A H10E 0.9800 . ?
C10A H10F 0.9800 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.517(3) . ?
C12 C13 1.392(3) . ?
C12 C17 1.396(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.394(3) . ?
C14 C15 1.392(3) . ?
C14 C18 1.538(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.398(3) . ?
C16 C17 1.389(3) . ?
C16 C22 1.526(2) . ?
C17 O2 1.391(2) . ?
C18 C19 1.541(3) . ?
C18 C20 1.527(3) . ?
C18 C21 1.535(3) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.528(2) . ?
C23 C24 1.388(3) . ?
C23 C28 1.399(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.402(3) . ?
C25 C26 1.392(3) . ?
C25 C29 1.533(3) . ?
C26 H26 0.9500 . ?
C26 C27 1.397(3) . ?
C27 C28 1.389(3) . ?
C27 C33 1.522(2) . ?
C28 O3 1.374(2) . ?
C29 C30 1.531(3) . ?
C29 C31 1.531(3) . ?
C29 C32 1.542(3) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.524(2) . ?
C34 C35 1.395(3) . ?
C34 C39 1.398(3) . ?
C35 H35 0.9500 . ?
C35 C36 1.394(3) . ?
C36 C37 1.396(3) . ?
C36 C40 1.533(3) . ?
C37 H37 0.9500 . ?
C37 C38 1.401(3) . ?
C38 C39 1.392(3) . ?
C38 C44 1.518(3) . ?
C39 O4 1.376(2) . ?
C40 C41 1.533(3) . ?
C40 C42 1.532(3) . ?
C40 C43 1.542(3) . ?
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 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C45 1.523(3) . ?
C45 C46 1.393(3) . ?
C45 C50 1.397(3) . ?
C46 C47 1.402(3) . ?
C46 O5 1.389(2) . ?
C47 C48 1.391(3) . ?
C47 C55 1.526(3) . ?
C48 H48 0.9500 . ?
C48 C49 1.398(3) . ?
C49 C50 1.394(3) . ?
C49 C51 1.538(3) . ?
C50 H50 0.9500 . ?
C51 C52 1.534(3) . ?
C51 C53 1.536(3) . ?
C51 C54 1.535(3) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C55 C56 1.524(3) . ?
C56 C57 1.392(3) . ?
C56 C61 1.402(3) . ?
C57 H57 0.9500 . ?
C57 C58 1.401(3) . ?
C58 C59 1.395(3) . ?
C58 C62 1.533(3) . ?
C59 H59 0.9500 . ?
C59 C60 1.395(3) . ?
C60 C61 1.390(3) . ?
C60 C66 1.521(2) . ?
C61 O6 1.385(2) . ?
C62 C63 1.534(3) . ?
C62 C64 1.534(3) . ?
C62 C65 1.532(3) . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
O1 H1 0.8400 . ?
O2 H2 0.8400 . ?
O3 H3A 0.8400 . ?
O4 H4 0.8400 . ?
O5 H5A 0.8400 . ?
O6 H6 0.8400 . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C67 Cl1A 1.748(17) . ?
C67 Cl2 1.742(18) . ?
C67A H67C 0.9900 . ?
C67A H67D 0.9900 . ?
C67A Cl1 1.755(3) . ?
C67A Cl2A 1.745(4) . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
C68 Cl4A 1.545(15) . ?
C68 Cl3A 1.449(10) . ?
C68A H68C 0.9900 . ?
C68A H68D 0.9900 . ?
C68A Cl4 1.812(6) . ?
C68A Cl3 1.740(4) . ?
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 -0.2(3) . . . . ?
C1 C2 C66 C60 -79.6(2) . . . . ?
C1 C6 C11 C12 -84.5(2) . . . . ?
C2 C1 C6 C5 -1.9(3) . . . . ?
C2 C1 C6 C11 178.84(17) . . . . ?
C2 C3 C4 C5 -1.8(3) . . . . ?
C2 C3 C4 C7 179.25(18) . . . . ?
C3 C2 C66 C60 101.9(2) . . . . ?
C3 C4 C5 C6 1.9(3) . . . . ?
C3 C4 C7 C8 -9.5(3) . . . . ?
C3 C4 C7 C8A -48.9(6) . . . . ?
C3 C4 C7 C9 -130.0(2) . . . . ?
C3 C4 C7 C9A -174.4(7) . . . . ?
C3 C4 C7 C10 112.3(2) . . . . ?
C3 C4 C7 C10A 64.6(6) . . . . ?
C4 C5 C6 C1 -0.1(3) . . . . ?
C4 C5 C6 C11 179.08(17) . . . . ?
C5 C4 C7 C8 171.6(2) . . . . ?
C5 C4 C7 C8A 132.2(6) . . . . ?
C5 C4 C7 C9 51.1(3) . . . . ?
C5 C4 C7 C9A 6.6(7) . . . . ?
C5 C4 C7 C10 -66.7(3) . . . . ?
C5 C4 C7 C10A -114.4(6) . . . . ?
C5 C6 C11 C12 96.3(2) . . . . ?
C6 C1 C2 C3 2.1(3) . . . . ?
C6 C1 C2 C66 -176.41(17) . . . . ?
C6 C11 C12 C13 -90.7(2) . . . . ?
C6 C11 C12 C17 91.2(2) . . . . ?
C7 C4 C5 C6 -179.05(17) . . . . ?
C11 C12 C13 C14 -177.97(17) . . . . ?
C11 C12 C17 C16 -179.61(17) . . . . ?
C11 C12 C17 O2 4.2(3) . . . . ?
C12 C13 C14 C15 -1.9(3) . . . . ?
C12 C13 C14 C18 176.48(17) . . . . ?
C13 C12 C17 C16 2.2(3) . . . . ?
C13 C12 C17 O2 -173.90(16) . . . . ?
C13 C14 C15 C16 1.3(3) . . . . ?
C13 C14 C18 C19 -61.6(2) . . . . ?
C13 C14 C18 C20 178.17(17) . . . . ?
C13 C14 C18 C21 58.6(2) . . . . ?
C14 C15 C16 C17 1.0(3) . . . . ?
C14 C15 C16 C22 179.31(17) . . . . ?
C15 C14 C18 C19 116.7(2) . . . . ?
C15 C14 C18 C20 -3.5(3) . . . . ?
C15 C14 C18 C21 -123.08(19) . . . . ?
C15 C16 C17 C12 -2.8(3) . . . . ?
C15 C16 C17 O2 173.37(16) . . . . ?
C15 C16 C22 C23 91.3(2) . . . . ?
C16 C22 C23 C24 -101.5(2) . . . . ?
C16 C22 C23 C28 77.2(2) . . . . ?
C17 C12 C13 C14 0.2(3) . . . . ?
C17 C16 C22 C23 -90.4(2) . . . . ?
C18 C14 C15 C16 -177.04(17) . . . . ?
C22 C16 C17 C12 178.88(17) . . . . ?
C22 C16 C17 O2 -4.9(3) . . . . ?
C22 C23 C24 C25 177.87(17) . . . . ?
C22 C23 C28 C27 -177.43(17) . . . . ?
C22 C23 C28 O3 3.1(3) . . . . ?
C23 C24 C25 C26 0.4(3) . . . . ?
C23 C24 C25 C29 -178.64(18) . . . . ?
C24 C23 C28 C27 1.4(3) . . . . ?
C24 C23 C28 O3 -178.15(17) . . . . ?
C24 C25 C26 C27 -0.3(3) . . . . ?
C24 C25 C29 C30 -61.8(2) . . . . ?
C24 C25 C29 C31 176.97(18) . . . . ?
C24 C25 C29 C32 57.8(2) . . . . ?
C25 C26 C27 C28 0.7(3) . . . . ?
C25 C26 C27 C33 -176.52(17) . . . . ?
C26 C25 C29 C30 119.2(2) . . . . ?
C26 C25 C29 C31 -2.0(3) . . . . ?
C26 C25 C29 C32 -121.2(2) . . . . ?
C26 C27 C28 C23 -1.2(3) . . . . ?
C26 C27 C28 O3 178.29(16) . . . . ?
C26 C27 C33 C34 -90.8(2) . . . . ?
C27 C33 C34 C35 97.3(2) . . . . ?
C27 C33 C34 C39 -86.2(2) . . . . ?
C28 C23 C24 C25 -0.9(3) . . . . ?
C28 C27 C33 C34 92.1(2) . . . . ?
C29 C25 C26 C27 178.75(18) . . . . ?
C33 C27 C28 C23 175.96(17) . . . . ?
C33 C27 C28 O3 -4.5(3) . . . . ?
C33 C34 C35 C36 175.71(17) . . . . ?
C33 C34 C39 C38 -173.24(17) . . . . ?
C33 C34 C39 O4 3.7(3) . . . . ?
C34 C35 C36 C37 -1.1(3) . . . . ?
C34 C35 C36 C40 179.68(18) . . . . ?
C35 C34 C39 C38 3.3(3) . . . . ?
C35 C34 C39 O4 -179.71(16) . . . . ?
C35 C36 C37 C38 0.9(3) . . . . ?
C35 C36 C40 C41 -58.4(2) . . . . ?
C35 C36 C40 C42 -178.96(18) . . . . ?
C35 C36 C40 C43 61.4(2) . . . . ?
C36 C37 C38 C39 1.3(3) . . . . ?
C36 C37 C38 C44 -176.40(17) . . . . ?
C37 C36 C40 C41 122.4(2) . . . . ?
C37 C36 C40 C42 1.9(3) . . . . ?
C37 C36 C40 C43 -117.7(2) . . . . ?
C37 C38 C39 C34 -3.5(3) . . . . ?
C37 C38 C39 O4 179.43(16) . . . . ?
C37 C38 C44 C45 99.1(2) . . . . ?
C38 C44 C45 C46 97.3(2) . . . . ?
C38 C44 C45 C50 -80.6(2) . . . . ?
C39 C34 C35 C36 -1.0(3) . . . . ?
C39 C38 C44 C45 -78.5(2) . . . . ?
C40 C36 C37 C38 -179.87(18) . . . . ?
C44 C38 C39 C34 174.22(17) . . . . ?
C44 C38 C39 O4 -2.9(3) . . . . ?
C44 C45 C46 C47 -177.82(17) . . . . ?
C44 C45 C46 O5 1.8(3) . . . . ?
C44 C45 C50 C49 177.04(18) . . . . ?
C45 C46 C47 C48 0.2(3) . . . . ?
C45 C46 C47 C55 -179.03(17) . . . . ?
C46 C45 C50 C49 -1.0(3) . . . . ?
C46 C47 C48 C49 0.3(3) . . . . ?
C46 C47 C55 C56 -100.3(2) . . . . ?
C47 C48 C49 C50 -1.1(3) . . . . ?
C47 C48 C49 C51 179.76(18) . . . . ?
C47 C55 C56 C57 -116.4(2) . . . . ?
C47 C55 C56 C61 66.0(2) . . . . ?
C48 C47 C55 C56 80.5(2) . . . . ?
C48 C49 C50 C45 1.5(3) . . . . ?
C48 C49 C51 C52 -55.4(2) . . . . ?
C48 C49 C51 C53 -175.3(2) . . . . ?
C48 C49 C51 C54 64.6(2) . . . . ?
C50 C45 C46 C47 0.1(3) . . . . ?
C50 C45 C46 O5 179.77(16) . . . . ?
C50 C49 C51 C52 125.5(2) . . . . ?
C50 C49 C51 C53 5.6(3) . . . . ?
C50 C49 C51 C54 -114.5(2) . . . . ?
C51 C49 C50 C45 -179.41(18) . . . . ?
C55 C47 C48 C49 179.54(18) . . . . ?
C55 C56 C57 C58 -178.01(17) . . . . ?
C55 C56 C61 C60 -177.41(17) . . . . ?
C55 C56 C61 O6 2.6(3) . . . . ?
C56 C57 C58 C59 -3.6(3) . . . . ?
C56 C57 C58 C62 174.91(17) . . . . ?
C57 C56 C61 C60 5.0(3) . . . . ?
C57 C56 C61 O6 -175.01(16) . . . . ?
C57 C58 C59 C60 3.1(3) . . . . ?
C57 C58 C62 C63 57.9(2) . . . . ?
C57 C58 C62 C64 -61.1(2) . . . . ?
C57 C58 C62 C65 178.83(18) . . . . ?
C58 C59 C60 C61 1.1(3) . . . . ?
C58 C59 C60 C66 -178.08(17) . . . . ?
C59 C58 C62 C63 -123.7(2) . . . . ?
C59 C58 C62 C64 117.3(2) . . . . ?
C59 C58 C62 C65 -2.8(3) . . . . ?
C59 C60 C61 C56 -5.4(3) . . . . ?
C59 C60 C61 O6 174.61(16) . . . . ?
C59 C60 C66 C2 -80.0(2) . . . . ?
C61 C56 C57 C58 -0.4(3) . . . . ?
C61 C60 C66 C2 100.8(2) . . . . ?
C62 C58 C59 C60 -175.28(17) . . . . ?
C66 C2 C3 C4 178.34(17) . . . . ?
C66 C60 C61 C56 173.86(17) . . . . ?
C66 C60 C61 O6 -6.2(3) . . . . ?
O1 C1 C2 C3 -177.71(17) . . . . ?
O1 C1 C2 C66 3.8(3) . . . . ?
O1 C1 C6 C5 177.88(16) . . . . ?
O1 C1 C6 C11 -1.3(3) . . . . ?
O5 C46 C47 C48 -179.44(16) . . . . ?
O5 C46 C47 C55 1.3(3) . . . . ?
