#------------------------------------------------------------------------------
#$Date: 2020-04-28 22:49:32 +0300 (Tue, 28 Apr 2020) $
#$Revision: 251222 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/48/4134805.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_4134805
loop_
_publ_author_name
'Han, Xiao-Ni'
'Han, Ying'
'Chen, Chuan-Feng'
_publ_section_title
;
 Pagoda[4]arene and i-Pagoda[4]arene.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c00624
_journal_year                    2020
_chemical_formula_moiety         '2(C H2 Cl2), C68 H56 O8'
_chemical_formula_sum            'C70 H60 Cl4 O8'
_chemical_formula_weight         1170.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.1490(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.3783(2)
_cell_length_b                   23.7901(2)
_cell_length_c                   10.94360(10)
_cell_measurement_reflns_used    13239
_cell_measurement_temperature    169.99(14)
_cell_measurement_theta_max      72.7670
_cell_measurement_theta_min      2.7170
_cell_volume                     5735.01(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -49.00 -23.00   0.50    0.52    --  -47.20 108.00 125.00   52
  2  ω     24.00  86.00   0.50    0.52    --   47.20-108.00  28.00  124
  3  ω   -148.00-123.00   0.50    2.08    --  -99.00-108.00  28.00   50
  4  ω    -92.00 -67.00   0.50    2.08    --  -99.00 108.00 125.00   50
  5  ω     87.00 163.00   0.50    2.08    --  103.25 108.00 125.00  152
  6  ω     65.00 108.00   0.50    2.08    --  103.25-108.00  28.00   86
  7  ω   -119.00 -80.00   0.50    0.52    --  -47.20-125.00 -90.00   78
  8  ω   -109.00 -82.00   0.50    0.52    --  -47.20-125.00  90.00   54
  9  ω   -110.00 -83.00   0.50    0.52    --  -47.20-125.00-120.00   54
 10  ω     26.00 120.00   0.50    0.52    --   47.20  77.00 120.00  188
 11  ω    -88.00 -37.00   0.50    2.08    --  -99.00  30.00 150.00  102
 12  ω   -165.00 -83.00   0.50    2.08    --  -99.00 -61.00 -60.00  164
 13  ω    -97.00 -26.00   0.50    2.08    --  -99.00  77.00-180.00  142
 14  ω   -161.00-133.00   0.50    2.08    --  -99.00 -77.00  60.00   56
 15  ω   -117.00 -77.00   0.50    2.08    --  -99.00 -77.00  60.00   80
 16  ω     31.00 106.00   0.50    2.08    --  103.25 -94.00-150.00  150
 17  ω     43.00 100.00   0.50    2.08    --  103.25 -94.00-180.00  114
 18  ω     31.00  42.00   0.50    2.08    --  103.25 -94.00  60.00   22
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0166157000
_diffrn_orient_matrix_UB_12      0.0140998000
_diffrn_orient_matrix_UB_13      0.1272839000
_diffrn_orient_matrix_UB_21      -0.0120448000
_diffrn_orient_matrix_UB_22      0.0614950000
_diffrn_orient_matrix_UB_23      -0.0412026000
_diffrn_orient_matrix_UB_31      -0.0668714000
_diffrn_orient_matrix_UB_32      -0.0145407000
_diffrn_orient_matrix_UB_33      -0.0504902000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            34797
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.421
_diffrn_reflns_theta_min         2.734
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.352
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       needle
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.158
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     747
_refine_ls_number_reflns         11002
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0930
_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)+(0.1664P)²+7.2994P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2568
_refine_ls_wR_factor_ref         0.2723
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9208
_reflns_number_total             11002
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja0c00624_si_005.cif
_cod_data_source_block           tx1582a
_cod_database_code               4134805
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHOCl
_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.
;
_reflns_odcompleteness_completeness 98.25
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Secondary CH2 refined with riding coordinates:
 C69(H69A,H69B), C70(H70A,H70B), C17(H17A,H17B), C34(H34A,H34B), C51(H51A,
 H51B), C68(H68A,H68B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C9(H9), C10(H10), C12(H12), C20(H20), C21(H21),
 C23(H23), C27(H27), C28(H28), C30(H30), C37(H37), C39(H39), C40(H40), C44(H44),
  C46(H46), C47(H47), C54(H54), C56(H56), C57(H57), C61(H61), C63(H63), C64(H64)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C66(H66A,H66B,H66C), C67(H67A,
 H67B,H67C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.436
_oxdiff_exptl_absorpt_empirical_full_min 0.721
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Cl1 Cl 0.24301(10) 0.54995(6) 0.35708(18) 0.1106(6) Uani 1 1 d . . . . .
Cl2 Cl 0.15566(8) 0.50150(7) 0.49044(18) 0.0993(5) Uani 1 1 d . . . . .
C69 C 0.2031(3) 0.4900(3) 0.3845(7) 0.0929(18) Uani 1 1 d . . . . .
H69A H 0.179176 0.477187 0.306863 0.112 Uiso 1 1 calc R . . . .
H69B H 0.231721 0.460432 0.415336 0.112 Uiso 1 1 calc R . . . .
Cl3 Cl 0.26812(7) 0.43686(5) 0.13469(14) 0.0779(4) Uani 1 1 d . . . . .
Cl4 Cl 0.32680(10) 0.49604(6) -0.04285(18) 0.1083(6) Uani 1 1 d . . . . .
C70 C 0.2920(2) 0.50234(19) 0.0883(5) 0.0659(12) Uani 1 1 d . . . . .
H70A H 0.320391 0.518859 0.155889 0.079 Uiso 1 1 calc R . . . .
H70B H 0.257226 0.527232 0.069322 0.079 Uiso 1 1 calc R . . . .
O1 O 0.41596(12) 0.67874(9) 0.6021(2) 0.0435(6) Uani 1 1 d . . . . .
O2 O 0.40313(12) 0.27809(10) 0.3007(3) 0.0502(6) Uani 1 1 d . . . . .
O3 O 0.50971(10) 0.60607(10) 0.1975(2) 0.0417(5) Uani 1 1 d . . . . .
O4 O 0.07384(12) 0.70054(12) 0.2146(3) 0.0613(8) Uani 1 1 d . . . . .
O5 O 0.17958(13) 0.64853(12) -0.2006(3) 0.0567(7) Uani 1 1 d . . . . .
O6 O -0.01175(12) 0.38189(11) 0.3284(2) 0.0471(6) Uani 1 1 d . . . . .
O7 O 0.07062(11) 0.31939(11) -0.0959(2) 0.0467(6) Uani 1 1 d . . . . .
O8 O 0.33475(12) 0.35145(12) 0.7438(2) 0.0503(6) Uani 1 1 d . . . . .
C1 C 0.40780(16) 0.62169(14) 0.5874(3) 0.0395(7) Uani 1 1 d . . . . .
C2 C 0.38185(19) 0.58963(16) 0.6733(3) 0.0482(8) Uani 1 1 d . . . . .
H2 H 0.370362 0.607168 0.741473 0.058 Uiso 1 1 calc R . . . .
C3 C 0.37352(19) 0.53332(16) 0.6571(3) 0.0485(9) Uani 1 1 d . . . . .
H3 H 0.356104 0.512834 0.714113 0.058 Uiso 1 1 calc R . . . .
C4 C 0.39107(16) 0.50525(14) 0.5540(3) 0.0386(7) Uani 1 1 d . . . . .
C5 C 0.38323(15) 0.44713(13) 0.5374(3) 0.0356(7) Uani 1 1 d . . . . .
H5 H 0.366179 0.426624 0.594923 0.043 Uiso 1 1 calc R . . . .
C6 C 0.40019(14) 0.41938(13) 0.4375(3) 0.0331(6) Uani 1 1 d . . . . .
C7 C 0.39192(14) 0.35933(13) 0.4213(3) 0.0349(7) Uani 1 1 d . . . . .
C8 C 0.41225(15) 0.33476(14) 0.3225(3) 0.0407(7) Uani 1 1 d . . . . .
C9 C 0.43939(17) 0.36665(15) 0.2367(3) 0.0450(8) Uani 1 1 d . . . . .
H9 H 0.452127 0.348720 0.170214 0.054 Uiso 1 1 calc R . . . .
C10 C 0.44681(16) 0.42300(15) 0.2511(3) 0.0421(7) Uani 1 1 d . . . . .
H10 H 0.464618 0.443206 0.194214 0.051 Uiso 1 1 calc R . . . .
C11 C 0.42776(14) 0.45190(14) 0.3521(3) 0.0359(7) Uani 1 1 d . . . . .
C12 C 0.43615(14) 0.50964(14) 0.3692(3) 0.0356(7) Uani 1 1 d . . . . .
H12 H 0.454455 0.529811 0.313006 0.043 Uiso 1 1 calc R . . . .
C13 C 0.41800(14) 0.53804(13) 0.4677(3) 0.0343(6) Uani 1 1 d . . . . .
C14 C 0.42536(15) 0.59777(13) 0.4842(3) 0.0356(7) Uani 1 1 d . . . . .
C15 C 0.3910(2) 0.70652(17) 0.6967(4) 0.0598(11) Uani 1 1 d . . . . .
H15A H 0.348773 0.697171 0.688776 0.090 Uiso 1 1 calc GR . . . .
H15B H 0.395284 0.746425 0.688476 0.090 Uiso 1 1 calc GR . . . .
H15C H 0.412142 0.694709 0.776587 0.090 Uiso 1 1 calc GR . . . .
C16 C 0.45470(18) 0.24533(17) 0.3064(5) 0.0674(13) Uani 1 1 d . . . . .
H16A H 0.475704 0.255907 0.240596 0.101 Uiso 1 1 calc GR . . . .
H16B H 0.443306 0.206445 0.297527 0.101 Uiso 1 1 calc GR . . . .
H16C H 0.480848 0.250937 0.384916 0.101 Uiso 1 1 calc GR . . . .
C17 C 0.45342(14) 0.63353(13) 0.3953(3) 0.0332(6) Uani 1 1 d . . . . .
H17A H 0.494370 0.620069 0.395718 0.040 Uiso 1 1 calc R . . . .
H17B H 0.456602 0.671712 0.426881 0.040 Uiso 1 1 calc R . . . .
C18 C 0.42042(14) 0.63521(13) 0.2615(3) 0.0347(6) Uani 1 1 d . . . . .
C19 C 0.45023(15) 0.62178(14) 0.1662(3) 0.0395(7) Uani 1 1 d . . . . .
C20 C 0.42087(17) 0.62467(18) 0.0404(3) 0.0487(8) Uani 1 1 d . . . . .
H20 H 0.442642 0.617100 -0.022682 0.058 Uiso 1 1 calc R . . . .
C21 C 0.36118(17) 0.63840(19) 0.0116(3) 0.0505(9) Uani 1 1 d . . . . .
H21 H 0.342512 0.639636 -0.071337 0.061 Uiso 1 1 calc R . . . .
C22 C 0.32658(16) 0.65094(14) 0.1052(3) 0.0399(7) Uani 1 1 d . . . . .
C23 C 0.26384(16) 0.66168(15) 0.0774(3) 0.0433(8) Uani 1 1 d . . . . .
H23 H 0.244346 0.660829 -0.005017 0.052 Uiso 1 1 calc R . . . .
C24 C 0.23048(14) 0.67340(13) 0.1684(3) 0.0375(7) Uani 1 1 d . . . . .
C25 C 0.16480(16) 0.67894(14) 0.1403(4) 0.0436(8) Uani 1 1 d . . . . .
C26 C 0.13617(16) 0.69401(15) 0.2356(4) 0.0488(9) Uani 1 1 d . . . . .
C27 C 0.16733(17) 0.70191(16) 0.3592(4) 0.0518(9) Uani 1 1 d . . . . .
H27 H 0.145758 0.711450 0.421451 0.062 Uiso 1 1 calc R . . . .
C28 C 0.22858(17) 0.69557(16) 0.3866(4) 0.0490(9) Uani 1 1 d . . . . .
H28 H 0.248606 0.701300 0.467616 0.059 Uiso 1 1 calc R . . . .
C29 C 0.26281(16) 0.68019(13) 0.2926(3) 0.0395(7) Uani 1 1 d . . . . .
C30 C 0.32499(16) 0.66950(14) 0.3204(3) 0.0391(7) Uani 1 1 d . . . . .
H30 H 0.345193 0.674428 0.401532 0.047 Uiso 1 1 calc R . . . .
C31 C 0.35774(14) 0.65174(13) 0.2309(3) 0.0364(7) Uani 1 1 d . . . . .
C32 C 0.0535(2) 0.7543(2) 0.2018(7) 0.094(2) Uani 1 1 d . . . . .
H32A H 0.072878 0.773425 0.141946 0.141 Uiso 1 1 calc GR . . . .
H32B H 0.063000 0.773291 0.280250 0.141 Uiso 1 1 calc GR . . . .
H32C H 0.010380 0.754388 0.174036 0.141 Uiso 1 1 calc GR . . . .
C33 C 0.5372(2) 0.5765(2) 0.1106(4) 0.0582(10) Uani 1 1 d . . . . .
H33A H 0.542076 0.601053 0.043592 0.087 Uiso 1 1 calc GR . . . .
H33B H 0.511943 0.545247 0.078822 0.087 Uiso 1 1 calc GR . . . .
H33C H 0.576174 0.562867 0.150317 0.087 Uiso 1 1 calc GR . . . .
C34 C 0.13026(15) 0.66891(14) 0.0093(4) 0.0437(8) Uani 1 1 d . . . . .
H34A H 0.087798 0.677544 0.008054 0.052 Uiso 1 1 calc R . . . .
H34B H 0.145189 0.695190 -0.046045 0.052 Uiso 1 1 calc R . . . .
C35 C 0.13436(16) 0.61045(15) -0.0416(3) 0.0441(8) Uani 1 1 d . . . . .
C36 C 0.10962(15) 0.56241(14) 0.0120(3) 0.0419(8) Uani 1 1 d . . . . .
C37 C 0.07835(16) 0.56776(15) 0.1116(3) 0.0430(8) Uani 1 1 d . . . . .
H37 H 0.073394 0.603327 0.143631 0.052 Uiso 1 1 calc R . . . .
C38 C 0.05457(15) 0.52159(15) 0.1638(3) 0.0403(7) Uani 1 1 d . . . . .
C39 C 0.02192(17) 0.52771(16) 0.2628(3) 0.0463(8) Uani 1 1 d . . . . .
H39 H 0.015395 0.563609 0.291429 0.056 Uiso 1 1 calc R . . . .
C40 C -0.00004(17) 0.48296(16) 0.3169(3) 0.0452(8) Uani 1 1 d . . . . .
H40 H -0.021109 0.488229 0.382011 0.054 Uiso 1 1 calc R . . . .
C41 C 0.00923(15) 0.42770(15) 0.2737(3) 0.0408(7) Uani 1 1 d . . . . .
C42 C 0.03832(14) 0.41817(14) 0.1754(3) 0.0358(7) Uani 1 1 d . . . . .
C43 C 0.06118(14) 0.46630(14) 0.1171(3) 0.0359(7) Uani 1 1 d . . . . .
C44 C 0.08993(15) 0.46073(14) 0.0163(3) 0.0390(7) Uani 1 1 d . . . . .
H44 H 0.093179 0.425134 -0.016990 0.047 Uiso 1 1 calc R . . . .
C45 C 0.11446(15) 0.50668(16) -0.0378(3) 0.0409(7) Uani 1 1 d . . . . .
C46 C 0.14371(18) 0.50158(17) -0.1409(4) 0.0496(9) Uani 1 1 d . . . . .
H46 H 0.148246 0.466054 -0.173556 0.059 Uiso 1 1 calc R . . . .
C47 C 0.16567(19) 0.54721(19) -0.1946(4) 0.0543(9) Uani 1 1 d . . . . .
H47 H 0.184540 0.542680 -0.263192 0.065 Uiso 1 1 calc R . . . .
C48 C 0.15946(16) 0.60157(17) -0.1450(4) 0.0479(9) Uani 1 1 d . . . . .
C49 C -0.0253(3) 0.3882(2) 0.4497(4) 0.0711(13) Uani 1 1 d . . . . .
H49A H -0.061686 0.410098 0.445588 0.107 Uiso 1 1 calc GR . . . .
H49B H 0.007710 0.407001 0.501629 0.107 Uiso 1 1 calc GR . . . .
H49C H -0.031220 0.351868 0.483700 0.107 Uiso 1 1 calc GR . . . .
C50 C 0.2059(3) 0.6441(3) -0.3060(5) 0.0829(16) Uani 1 1 d . . . . .
H50A H 0.177141 0.628179 -0.372477 0.124 Uiso 1 1 calc GR . . . .
H50B H 0.241019 0.620272 -0.288692 0.124 Uiso 1 1 calc GR . . . .
H50C H 0.217770 0.680713 -0.329729 0.124 Uiso 1 1 calc GR . . . .
C51 C 0.04272(14) 0.35916(13) 0.1242(3) 0.0337(6) Uani 1 1 d . . . . .
H51A H 0.024211 0.333572 0.175634 0.040 Uiso 1 1 calc R . . . .
H51B H 0.018195 0.358113 0.041806 0.040 Uiso 1 1 calc R . . . .
C52 C 0.10482(15) 0.33618(13) 0.1149(3) 0.0358(7) Uani 1 1 d . . . . .
C53 C 0.15286(15) 0.33320(13) 0.2212(3) 0.0352(7) Uani 1 1 d . . . . .
C54 C 0.14359(15) 0.34825(14) 0.3398(3) 0.0397(7) Uani 1 1 d . . . . .
H54 H 0.104930 0.358771 0.351252 0.048 Uiso 1 1 calc R . . . .
C55 C 0.19111(16) 0.34787(15) 0.4419(3) 0.0403(7) Uani 1 1 d . . . . .
C56 C 0.18134(18) 0.3619(2) 0.5638(3) 0.0532(10) Uani 1 1 d . . . . .
H56 H 0.142451 0.371214 0.575925 0.064 Uiso 1 1 calc R . . . .
C57 C 0.22740(18) 0.3619(2) 0.6615(4) 0.0541(10) Uani 1 1 d . . . . .
H57 H 0.219831 0.370466 0.740297 0.065 Uiso 1 1 calc R . . . .
C58 C 0.28770(16) 0.34896(16) 0.6448(3) 0.0434(8) Uani 1 1 d . . . . .
C59 C 0.30118(15) 0.33658(14) 0.5303(3) 0.0382(7) Uani 1 1 d . . . . .
C60 C 0.25176(15) 0.33338(13) 0.4265(3) 0.0358(7) Uani 1 1 d . . . . .
C61 C 0.25938(15) 0.31502(13) 0.3101(3) 0.0377(7) Uani 1 1 d . . . . .
H61 H 0.297617 0.302944 0.299231 0.045 Uiso 1 1 calc R . . . .
C62 C 0.21202(15) 0.31395(13) 0.2088(3) 0.0369(7) Uani 1 1 d . . . . .
C63 C 0.22062(16) 0.29468(14) 0.0899(3) 0.0411(7) Uani 1 1 d . . . . .
H63 H 0.258522 0.281279 0.080010 0.049 Uiso 1 1 calc R . . . .
C64 C 0.17486(17) 0.29545(15) -0.0091(3) 0.0435(8) Uani 1 1 d . . . . .
H64 H 0.181336 0.281888 -0.085429 0.052 Uiso 1 1 calc R . . . .
C65 C 0.11680(16) 0.31697(14) 0.0032(3) 0.0400(7) Uani 1 1 d . . . . .
C66 C 0.32098(18) 0.34006(18) 0.8636(3) 0.0491(9) Uani 1 1 d . . . . .
H66A H 0.296679 0.306653 0.860017 0.074 Uiso 1 1 calc GR . . . .
H66B H 0.298966 0.371163 0.889707 0.074 Uiso 1 1 calc GR . . . .
H66C H 0.358007 0.334700 0.921663 0.074 Uiso 1 1 calc GR . . . .
C67 C 0.0833(2) 0.3164(2) -0.2170(4) 0.0650(12) Uani 1 1 d . . . . .
H67A H 0.046859 0.323816 -0.275665 0.097 Uiso 1 1 calc GR . . . .
H67B H 0.098017 0.279566 -0.231469 0.097 Uiso 1 1 calc GR . . . .
H67C H 0.113507 0.343881 -0.226739 0.097 Uiso 1 1 calc GR . . . .
C68 C 0.36590(14) 0.32416(13) 0.5155(3) 0.0363(7) Uani 1 1 d . . . . .
H68A H 0.368181 0.284931 0.492620 0.044 Uiso 1 1 calc R . . . .
H68B H 0.391802 0.328962 0.595776 0.044 Uiso 1 1 calc R . . . .
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
Cl2 C69 Cl1 112.4(3) . . ?
Cl3 C70 Cl4 111.3(3) . . ?
C1 O1 C15 118.9(3) . . ?
C8 O2 C16 116.5(3) . . ?
C19 O3 C33 119.3(3) . . ?
C32 O4 C26 115.7(3) . . ?
C48 O5 C50 121.5(4) . . ?
C41 O6 C49 118.1(3) . . ?
C65 O7 C67 119.9(3) . . ?
C58 O8 C66 117.3(3) . . ?
O1 C1 C2 121.1(3) . . ?
O1 C1 C14 116.8(3) . . ?
C14 C1 C2 122.0(3) . . ?
C3 C2 C1 120.5(3) . . ?
C2 C3 C4 121.0(3) . . ?
C3 C4 C13 118.2(3) . . ?
C5 C4 C3 121.3(3) . . ?
C5 C4 C13 120.5(3) . . ?
C6 C5 C4 121.8(3) . . ?
C5 C6 C7 121.3(3) . . ?
C5 C6 C11 117.8(3) . . ?
C11 C6 C7 120.9(3) . . ?
C6 C7 C68 121.0(3) . . ?
C8 C7 C6 117.6(3) . . ?
C8 C7 C68 121.2(3) . . ?
O2 C8 C9 118.4(3) . . ?
C7 C8 O2 119.5(3) . . ?
C7 C8 C9 122.1(3) . . ?
C10 C9 C8 120.5(3) . . ?
C9 C10 C11 121.2(3) . . ?
C10 C11 C6 117.8(3) . . ?
C12 C11 C6 120.5(3) . . ?
C12 C11 C10 121.7(3) . . ?
C13 C12 C11 122.1(3) . . ?
C4 C13 C14 120.4(3) . . ?
C12 C13 C4 117.3(3) . . ?
C12 C13 C14 122.3(3) . . ?
C1 C14 C13 117.8(3) . . ?
C1 C14 C17 120.3(3) . . ?
C13 C14 C17 121.8(3) . . ?
C14 C17 C18 116.7(2) . . ?
C19 C18 C17 120.5(3) . . ?
C19 C18 C31 118.2(3) . . ?
C31 C18 C17 121.3(3) . . ?
O3 C19 C18 117.1(3) . . ?
O3 C19 C20 121.4(3) . . ?
C18 C19 C20 121.5(3) . . ?
C21 C20 C19 120.4(3) . . ?
C20 C21 C22 121.5(3) . . ?
C21 C22 C31 117.5(3) . . ?
C23 C22 C21 122.2(3) . . ?
C23 C22 C31 120.3(3) . . ?
C24 C23 C22 121.9(3) . . ?
C23 C24 C25 121.5(3) . . ?
C23 C24 C29 117.6(3) . . ?
C29 C24 C25 120.9(3) . . ?
C24 C25 C34 120.8(3) . . ?
C26 C25 C24 117.1(3) . . ?
C26 C25 C34 122.1(3) . . ?
O4 C26 C27 117.1(4) . . ?
C25 C26 O4 119.9(4) . . ?
C25 C26 C27 123.0(3) . . ?
C28 C27 C26 120.2(4) . . ?
C27 C28 C29 121.0(4) . . ?
C24 C29 C28 117.7(3) . . ?
C30 C29 C24 120.3(3) . . ?
C30 C29 C28 121.9(3) . . ?
C31 C30 C29 122.2(3) . . ?
C22 C31 C18 120.7(3) . . ?
C30 C31 C18 122.3(3) . . ?
C30 C31 C22 117.0(3) . . ?
C35 C34 C25 116.0(3) . . ?
C36 C35 C34 121.9(3) . . ?
C48 C35 C34 120.7(3) . . ?
C48 C35 C36 117.3(3) . . ?
C35 C36 C45 121.0(3) . . ?
C37 C36 C35 121.7(3) . . ?
C37 C36 C45 117.2(3) . . ?
C38 C37 C36 121.9(3) . . ?
C37 C38 C39 121.4(3) . . ?
C37 C38 C43 120.7(3) . . ?
C39 C38 C43 117.9(3) . . ?
C40 C39 C38 122.0(4) . . ?
C39 C40 C41 119.7(3) . . ?
O6 C41 C40 120.6(3) . . ?
O6 C41 C42 117.4(3) . . ?
C42 C41 C40 122.0(3) . . ?
C41 C42 C43 118.0(3) . . ?
C41 C42 C51 120.8(3) . . ?
C43 C42 C51 121.1(3) . . ?
C38 C43 C42 120.2(3) . . ?
C44 C43 C38 117.9(3) . . ?
C44 C43 C42 121.9(3) . . ?
C43 C44 C45 122.5(3) . . ?
C44 C45 C36 119.7(3) . . ?
C44 C45 C46 123.0(3) . . ?
C46 C45 C36 117.3(3) . . ?
C47 C46 C45 122.0(4) . . ?
C46 C47 C48 119.5(4) . . ?
O5 C48 C47 120.3(4) . . ?
C35 C48 O5 116.9(4) . . ?
C35 C48 C47 122.7(3) . . ?
C52 C51 C42 118.6(3) . . ?
C53 C52 C51 121.8(3) . . ?
C65 C52 C51 120.4(3) . . ?
C65 C52 C53 117.9(3) . . ?
C54 C53 C52 121.8(3) . . ?
C54 C53 C62 117.5(3) . . ?
C62 C53 C52 120.7(3) . . ?
C53 C54 C55 121.6(3) . . ?
C54 C55 C56 121.6(3) . . ?
C54 C55 C60 120.5(3) . . ?
C56 C55 C60 117.9(3) . . ?
C57 C56 C55 121.3(3) . . ?
C56 C57 C58 120.4(4) . . ?
O8 C58 C57 120.0(3) . . ?
C59 C58 O8 118.0(3) . . ?
C59 C58 C57 121.9(3) . . ?
C58 C59 C60 118.0(3) . . ?
C58 C59 C68 120.6(3) . . ?
C60 C59 C68 121.4(3) . . ?
C55 C60 C59 120.3(3) . . ?
C61 C60 C55 117.0(3) . . ?
C61 C60 C59 122.7(3) . . ?
C60 C61 C62 122.6(3) . . ?
C61 C62 C53 120.4(3) . . ?
C61 C62 C63 121.8(3) . . ?
C63 C62 C53 117.8(3) . . ?
C64 C63 C62 121.5(3) . . ?
C63 C64 C65 120.2(3) . . ?
O7 C65 C52 117.0(3) . . ?
O7 C65 C64 121.1(3) . . ?
C52 C65 C64 121.8(3) . . ?
C59 C68 C7 116.9(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
Cl1 C69 1.737(6) . ?
Cl2 C69 1.727(7) . ?
Cl3 C70 1.750(4) . ?
Cl4 C70 1.756(5) . ?
O1 C1 1.375(4) . ?
O1 C15 1.422(4) . ?
O2 C8 1.378(4) . ?
O2 C16 1.385(5) . ?
O3 C19 1.367(4) . ?
O3 C33 1.408(5) . ?
O4 C26 1.382(4) . ?
O4 C32 1.357(5) . ?
O5 C48 1.385(4) . ?
O5 C50 1.389(6) . ?
O6 C41 1.366(4) . ?
O6 C49 1.420(5) . ?
O7 C65 1.361(4) . ?
O7 C67 1.405(5) . ?
O8 C58 1.373(4) . ?
O8 C66 1.424(4) . ?
C1 C2 1.412(5) . ?
C1 C14 1.382(5) . ?
C2 C3 1.360(5) . ?
C3 C4 1.424(5) . ?
C4 C5 1.402(5) . ?
C4 C13 1.437(5) . ?
C5 C6 1.386(4) . ?
C6 C7 1.447(4) . ?
C6 C11 1.434(5) . ?
C7 C8 1.375(5) . ?
C7 C68 1.521(4) . ?
C8 C9 1.424(5) . ?
C9 C10 1.357(5) . ?
C10 C11 1.429(5) . ?
C11 C12 1.395(5) . ?
C12 C13 1.392(5) . ?
C13 C14 1.438(4) . ?
C14 C17 1.510(4) . ?
C17 C18 1.521(4) . ?
C18 C19 1.371(5) . ?
C18 C31 1.438(5) . ?
C19 C20 1.418(5) . ?
C20 C21 1.357(5) . ?
C21 C22 1.420(5) . ?
C22 C23 1.407(5) . ?
C22 C31 1.429(5) . ?
C23 C24 1.375(5) . ?
C24 C25 1.454(5) . ?
C24 C29 1.432(5) . ?
C25 C26 1.364(6) . ?
C25 C34 1.523(5) . ?
C26 C27 1.421(6) . ?
C27 C28 1.359(5) . ?
C28 C29 1.434(5) . ?
C29 C30 1.394(5) . ?
C30 C31 1.388(5) . ?
C34 C35 1.507(5) . ?
C35 C36 1.439(5) . ?
C35 C48 1.365(6) . ?
C36 C37 1.401(5) . ?
C36 C45 1.445(5) . ?
C37 C38 1.387(5) . ?
C38 C39 1.417(5) . ?
C38 C43 1.428(5) . ?
C39 C40 1.352(5) . ?
C40 C41 1.424(5) . ?
C41 C42 1.370(5) . ?
C42 C43 1.448(5) . ?
C42 C51 1.521(4) . ?
C43 C44 1.377(5) . ?
C44 C45 1.401(5) . ?
C45 C46 1.406(5) . ?
C46 C47 1.367(6) . ?
C47 C48 1.419(6) . ?
C51 C52 1.513(4) . ?
C52 C53 1.440(4) . ?
C52 C65 1.375(5) . ?
C53 C54 1.397(5) . ?
C53 C62 1.430(5) . ?
C54 C55 1.400(5) . ?
C55 C56 1.429(5) . ?
C55 C60 1.439(5) . ?
C56 C57 1.348(5) . ?
C57 C58 1.427(5) . ?
C58 C59 1.371(5) . ?
C59 C60 1.441(5) . ?
C59 C68 1.515(5) . ?
C60 C61 1.385(5) . ?
C61 C62 1.392(5) . ?
C62 C63 1.425(5) . ?
C63 C64 1.353(5) . ?
C64 C65 1.425(5) . ?
