#------------------------------------------------------------------------------
#$Date: 2023-10-06 02:52:12 +0300 (Fri, 06 Oct 2023) $
#$Revision: 286715 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/98/1569831.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_1569831
loop_
_publ_author_name
'Kamin, Ashlyn A.'
'Clayton, Tara D.'
'Otteson, Claire E.'
'Gannon, Paige M.'
'Krajewski, Sebastian'
'Kaminsky, Werner'
'Jasti, Ramesh'
'Xiao, Dianne J.'
_publ_section_title
;
 Synthesis and metalation of polycatechol nanohoops derived from
 fluorocycloparaphenylenes.
;
_journal_issue                   36
_journal_name_full               'Chemical science'
_journal_page_first              9724
_journal_page_last               9732
_journal_paper_doi               10.1039/d3sc03561a
_journal_volume                  14
_journal_year                    2023
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C76 H56 O4, C2 H Cl3 [+ solvent]'
_chemical_formula_sum            'C78 H57 Cl3 O4'
_chemical_formula_weight         1164.58
_chemical_name_common            tetramethoxy[12]cycloparaphenylene
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      43
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.5
_audit_creation_date             2023-04-17T15:09:29-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2023-05-23 deposited with the CCDC.	2023-08-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   57.683(4)
_cell_length_b                   12.1111(8)
_cell_length_c                   50.915(3)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.76
_cell_measurement_theta_min      2.47
_cell_measurement_wavelength     0.71073
_cell_volume                     35569(4)
_computing_cell_refinement       'SAINT V8.38A integration software'
_computing_data_collection       'Bruker APEX2 software'
_computing_data_reduction        'SORTAV (Blessing, 1995)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       'φ or ω oscillation scans'
_diffrn_orient_matrix_UB_11      0.08256
_diffrn_orient_matrix_UB_12      -0.00011
_diffrn_orient_matrix_UB_13      -0.000232
_diffrn_orient_matrix_UB_21      0.001018
_diffrn_orient_matrix_UB_22      -0.003096
_diffrn_orient_matrix_UB_23      0.017118
_diffrn_orient_matrix_UB_31      -0.000632
_diffrn_orient_matrix_UB_32      -0.019395
_diffrn_orient_matrix_UB_33      -0.002731
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1097
_diffrn_reflns_av_unetI/netI     0.09
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       68
_diffrn_reflns_limit_h_min       -68
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            101139
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.027
_diffrn_source                   'sealed x-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.139
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        SADABS-2016/2 - Bruker AXS area detector scaling and absorption correcti
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.87
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             9728
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: trichloroethylene/n-heptane'
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.43
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.6(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     786
_refine_ls_number_reflns         15535
_refine_ls_number_restraints     1003
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.18
_refine_ls_R_factor_gt           0.1202
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1793P)²+212.6177P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3064
_refine_ls_wR_factor_ref         0.3545
_reflns_Friedel_coverage         0.978
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                9099
_reflns_number_total             15535
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3sc03561a2.cif
_cod_data_source_block           AAK_4245_4_TCE_hept
_cod_depositor_comments
'Adding full bibliography for 1569828--1569831.cif.'
_cod_database_code               1569831
_shelx_estimated_absorpt_t_min   0.921
_shelx_estimated_absorpt_t_max   0.988
_shelx_shelxl_version_number     2014/7
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/4, y+1/4, z+1/4'
'x+3/4, -y+3/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/4, y+3/4, z+3/4'
'x+3/4, -y+5/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+3/4, y+1/4, z+3/4'
'x+5/4, -y+3/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+3/4, y+3/4, z+1/4'
'x+5/4, -y+5/4, z+1/4'
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 0.1277(2) 0.3990(9) 1.02213(12) 0.058(3) Uani 1 1 d D U . . .
C2 C 0.1157(2) 0.3180(9) 1.0360(2) 0.052(3) Uani 1 1 d . U . . .
C3 C 0.1156(2) 0.3222(9) 1.0633(3) 0.064(3) Uani 1 1 d . . . . .
C4 C 0.1274(2) 0.4019(9) 1.07715(13) 0.058(3) Uani 1 1 d D . . . .
C5 C 0.1391(2) 0.4826(10) 1.0629(3) 0.070(4) Uani 1 1 d . . . . .
C6 C 0.1393(2) 0.4814(9) 1.0361(3) 0.066(4) Uani 1 1 d . . . . .
C7 C 0.0816(3) 0.2637(12) 1.0136(3) 0.087(5) Uani 1 1 d . . . . .
H7A H 0.0747 0.1974 1.0057 0.13 Uiso 1 1 calc R U . . .
H7B H 0.0714 0.2909 1.0275 0.13 Uiso 1 1 calc R U . . .
H7C H 0.0833 0.3208 1.0001 0.13 Uiso 1 1 calc R U . . .
C8 C 0.0814(2) 0.2648(16) 1.0857(3) 0.100(6) Uani 1 1 d . . . . .
H8A H 0.074 0.2032 1.0949 0.15 Uiso 1 1 calc R U . . .
H8B H 0.0827 0.3281 1.0976 0.15 Uiso 1 1 calc R U . . .
H8C H 0.072 0.2855 1.0704 0.15 Uiso 1 1 calc R U . . .
C9 C 0.1696(4) 0.5565(19) 1.0860(4) 0.138(9) Uani 1 1 d . . . . .
H9A H 0.1746 0.6266 1.0937 0.206 Uiso 1 1 calc R U . . .
H9B H 0.1683 0.5005 1.0999 0.206 Uiso 1 1 calc R U . . .
H9C H 0.1809 0.5324 1.0729 0.206 Uiso 1 1 calc R U . . .
C10 C 0.1719(4) 0.578(2) 1.0163(5) 0.169(12) Uani 1 1 d . . . . .
H10A H 0.1742 0.6445 1.0055 0.253 Uiso 1 1 calc R U . . .
H10B H 0.1805 0.5862 1.0328 0.253 Uiso 1 1 calc R U . . .
H10C H 0.1777 0.5136 1.0068 0.253 Uiso 1 1 calc R U . . .
C11 C 0.12378(12) 0.4081(4) 1.10660(8) 0.049(3) Uani 1 1 d D . . . .
C12 C 0.12597(12) 0.3159(4) 1.12285(9) 0.056(3) Uani 1 1 d D U . . .
H12 H 0.1348 0.2544 1.117 0.067 Uiso 1 1 calc R U . . .
C13 C 0.11558(11) 0.3121(3) 1.14732(8) 0.045(3) Uani 1 1 d D . . . .
H13 H 0.1176 0.2491 1.1582 0.054 Uiso 1 1 calc R U . . .
C14 C 0.10209(10) 0.4000(4) 1.15621(8) 0.047(3) Uani 1 1 d D . . . .
C15 C 0.10113(13) 0.4944(4) 1.14069(9) 0.065(3) Uani 1 1 d D . . . .
H15 H 0.0929 0.5571 1.1469 0.079 Uiso 1 1 calc R U . . .
C16 C 0.11186(12) 0.4989(3) 1.11656(8) 0.063(3) Uani 1 1 d D . . . .
H16 H 0.1111 0.565 1.1065 0.076 Uiso 1 1 calc R U . . .
C17 C 0.08461(7) 0.3791(4) 1.17777(10) 0.056(3) Uani 1 1 d D . . . .
C18 C 0.08466(7) 0.2859(4) 1.19391(12) 0.068(4) Uani 1 1 d D . . . .
H18 H 0.0981 0.2405 1.1946 0.082 Uiso 1 1 calc R U . . .
C19 C 0.06558(8) 0.2583(4) 1.20900(13) 0.079(4) Uani 1 1 d D . . . .
H19 H 0.0659 0.1935 1.2195 0.094 Uiso 1 1 calc R U . . .
C20 C 0.04582(7) 0.3245(4) 1.20891(13) 0.068(4) Uani 1 1 d D . . . .
C21 C 0.04653(7) 0.4218(4) 1.19443(13) 0.071(4) Uani 1 1 d D . . . .
H21 H 0.0337 0.4711 1.1952 0.085 Uiso 1 1 calc R U . . .
C22 C 0.06536(8) 0.4483(4) 1.17905(12) 0.065(3) Uani 1 1 d D . . . .
H22 H 0.0652 0.5148 1.1691 0.077 Uiso 1 1 calc R U . . .
C23 C 0.02219(7) 0.2897(4) 1.2191(3) 0.059(3) Uani 0.379(14) 1 d D U P A 1
C24 C 0.01710(7) 0.1771(3) 1.2195(6) 0.058(5) Uani 0.379(14) 1 d D U P A 1
H24 H 0.0294 0.1251 1.219 0.069 Uiso 0.379(14) 1 calc R U P A 1
C25 C -0.00552(7) 0.1396(3) 1.2207(5) 0.059(5) Uani 0.379(14) 1 d D U P A 1
H25 H -0.0085 0.0625 1.2213 0.071 Uiso 0.379(14) 1 calc R U P A 1
C26 C -0.02399(6) 0.2138(4) 1.2210(3) 0.054(3) Uani 0.379(14) 1 d D U P A 1
C27 C -0.01880(7) 0.3257(4) 1.2225(6) 0.052(4) Uani 0.379(14) 1 d D U P A 1
H27 H -0.0311 0.3776 1.224 0.062 Uiso 0.379(14) 1 calc R U P A 1
C28 C 0.00375(7) 0.3630(3) 1.2218(5) 0.057(4) Uani 0.379(14) 1 d D U P A 1
H28 H 0.0068 0.4399 1.2233 0.068 Uiso 0.379(14) 1 calc R U P A 1
C23B C 0.02334(6) 0.2793(4) 1.21819(15) 0.059(3) Uani 0.621(14) 1 d D . P A 2
C24B C 0.01656(7) 0.1821(4) 1.20563(17) 0.058(5) Uani 0.621(14) 1 d D . P A 2
H24B H 0.0278 0.1395 1.1966 0.069 Uiso 0.621(14) 1 calc R U P A 2
C25B C -0.00622(7) 0.1465(4) 1.20612(19) 0.059(5) Uani 0.621(14) 1 d D . P A 2
H25B H -0.0101 0.077 1.1987 0.071 Uiso 0.621(14) 1 calc R U P A 2
C26B C -0.02348(6) 0.2117(4) 1.21738(16) 0.054(3) Uani 0.621(14) 1 d D . P A 2
C27B C -0.01675(7) 0.3094(5) 1.22954(17) 0.052(4) Uani 0.621(14) 1 d D . P A 2
H27B H -0.0281 0.353 1.2382 0.062 Uiso 0.621(14) 1 calc R U P A 2
C28B C 0.00597(7) 0.3443(4) 1.22923(18) 0.057(4) Uani 0.621(14) 1 d D . P A 2
H28B H 0.0099 0.4139 1.2367 0.068 Uiso 0.621(14) 1 calc R U P A 2
C29 C -0.04783(7) 0.1859(3) 1.20998(14) 0.060(3) Uani 1 1 d D . . . .
C30 C -0.05331(9) 0.0764(3) 1.20413(16) 0.101(5) Uani 1 1 d D . . . .
H30 H -0.0437 0.0189 1.2107 0.121 Uiso 1 1 calc R U . . .
C31 C -0.07241(10) 0.0499(3) 1.18897(15) 0.104(6) Uani 1 1 d D . . . .
H31 H -0.0757 -0.0253 1.1851 0.125 Uiso 1 1 calc R U . . .
C32 C -0.08690(9) 0.1323(3) 1.17924(12) 0.053(3) Uani 1 1 d D . . . .
C33 C -0.08254(9) 0.2404(3) 1.18701(14) 0.071(4) Uani 1 1 d D . . . .
H33 H -0.0929 0.2973 1.1819 0.086 Uiso 1 1 calc R U . . .
C34 C -0.06346(8) 0.2669(3) 1.20201(13) 0.057(3) Uani 1 1 d D . . . .
H34 H -0.0609 0.3415 1.207 0.068 Uiso 1 1 calc R U . . .
C35 C -0.10374(10) 0.1013(4) 1.15756(8) 0.049(3) Uani 1 1 d D U . . .
C36 C -0.10120(11) 0.0069(4) 1.14210(9) 0.056(3) Uani 1 1 d D U . . .
H36 H -0.0916 -0.0516 1.1482 0.067 Uiso 1 1 calc R U . . .
C37 C -0.11232(11) -0.0032(4) 1.11816(8) 0.056(3) Uani 1 1 d D U . . .
H37 H -0.1105 -0.0689 1.1082 0.067 Uiso 1 1 calc R U . . .
C38 C -0.12617(10) 0.0820(4) 1.10854(7) 0.044(2) Uani 1 1 d D U . . .
C39 C -0.12958(11) 0.1736(4) 1.12455(8) 0.051(3) Uani 1 1 d D U . . .
H39 H -0.1396 0.231 1.1188 0.062 Uiso 1 1 calc R U . . .
C40 C -0.11878(10) 0.1829(4) 1.14857(8) 0.045(3) Uani 1 1 d D U . . .
H40 H -0.1216 0.246 1.1592 0.053 Uiso 1 1 calc R U . . .
C41 C -0.13453(16) 0.0815(3) 1.08043(6) 0.053(3) Uani 1 1 d D U . . .
C42 C -0.13757(17) -0.0155(3) 1.06607(7) 0.062(3) Uani 1 1 d D . . . .
H42 H -0.1398 -0.0833 1.0751 0.074 Uiso 1 1 calc R U . . .
C43 C -0.13743(19) -0.0152(3) 1.03891(7) 0.060(3) Uani 1 1 d D . . . .
H43 H -0.1387 -0.0829 1.0296 0.072 Uiso 1 1 calc R U . . .
C44 C -0.13545(16) 0.0836(3) 1.02504(6) 0.053(3) Uani 1 1 d D . . . .
C45 C -0.13445(18) 0.1811(3) 1.03943(7) 0.060(3) Uani 1 1 d D . . . .
H45 H -0.1343 0.2498 1.0304 0.073 Uiso 1 1 calc R U . . .
C46 C -0.1336(2) 0.1803(3) 1.06646(7) 0.059(3) Uani 1 1 d D . . . .
H46 H -0.1324 0.2481 1.0757 0.071 Uiso 1 1 calc R U . . .
C47 C -0.12925(12) 0.0807(4) 0.99623(8) 0.052(3) Uani 1 1 d D . . . .
C48 C -0.11662(11) -0.0090(3) 0.98670(9) 0.046(3) Uani 1 1 d D . . . .
H48 H -0.1165 -0.0761 0.9964 0.056 Uiso 1 1 calc R U . . .
C49 C -0.10428(11) -0.0024(3) 0.96346(9) 0.049(3) Uani 1 1 d D . . . .
H49 H -0.0962 -0.0653 0.9572 0.059 Uiso 1 1 calc R U . . .
C50 C -0.10366(10) 0.0957(4) 0.94914(9) 0.047(3) Uani 1 1 d D . . . .
C51 C -0.11707(11) 0.1834(3) 0.95807(9) 0.058(3) Uani 1 1 d D U . . .
H51 H -0.1175 0.2498 0.9482 0.07 Uiso 1 1 calc R U . . .
C52 C -0.12972(11) 0.1760(3) 0.98095(9) 0.056(3) Uani 1 1 d D U . . .
H52 H -0.1389 0.237 0.9864 0.067 Uiso 1 1 calc R U . . .
C53 C -0.08597(7) 0.1054(4) 0.92762(11) 0.044(2) Uani 1 1 d D U . . .
C54 C -0.06574(8) 0.0423(4) 0.92732(13) 0.056(3) Uani 1 1 d D U . . .
H54 H -0.065 -0.023 0.9376 0.068 Uiso 1 1 calc R U . . .
C55 C -0.04679(7) 0.0726(4) 0.91232(12) 0.056(3) Uani 1 1 d D U . . .
H55 H -0.0332 0.0286 0.9127 0.067 Uiso 1 1 calc R U . . .
C56 C -0.04749(6) 0.1670(4) 0.89669(12) 0.048(3) Uani 1 1 d D U . . .
C57 C -0.06800(7) 0.2273(4) 0.89618(12) 0.044(2) Uani 1 1 d D U . . .
H57 H -0.0691 0.2899 0.885 0.053 Uiso 1 1 calc R U . . .
C58 C -0.08671(7) 0.1982(4) 0.91149(11) 0.046(3) Uani 1 1 d D U . . .
H58 H -0.1003 0.2422 0.911 0.055 Uiso 1 1 calc R U . . .
C59 C -0.02422(6) 0.2137(4) 0.89014(15) 0.081(4) Uani 1 1 d D U . . .
C60 C -0.01728(7) 0.3165(4) 0.89973(17) 0.081(4) Uani 1 1 d D U . . .
H60 H -0.0283 0.3624 0.9083 0.098 Uiso 1 1 calc R U . . .
C61 C 0.00532(7) 0.3530(4) 0.89710(18) 0.117(6) Uani 1 1 d D U . . .
H61 H 0.0095 0.4238 0.9035 0.14 Uiso 1 1 calc R U . . .
C62 C 0.02200(6) 0.2867(4) 0.88509(15) 0.095(5) Uani 1 1 d D . . . .
C63 C 0.01468(7) 0.1879(4) 0.87392(15) 0.081(4) Uani 1 1 d D . . . .
H63 H 0.0255 0.1443 0.8644 0.097 Uiso 1 1 calc R U . . .
C64 C -0.00786(7) 0.1519(4) 0.87642(16) 0.084(4) Uani 1 1 d D . . . .
H64 H -0.0123 0.0838 0.8687 0.1 Uiso 1 1 calc R U . . .
C65 C 0.04678(8) 0.3156(3) 0.89144(14) 0.072(4) Uani 1 1 d D . . . .
C66 C 0.06177(9) 0.2340(3) 0.90073(15) 0.094(5) Uani 1 1 d D . . . .
H66 H 0.0585 0.1587 0.897 0.113 Uiso 1 1 calc R U . . .
C67 C 0.08127(9) 0.2604(3) 0.91523(15) 0.092(5) Uani 1 1 d D . . . .
H67 H 0.0913 0.2034 0.9211 0.111 Uiso 1 1 calc R U . . .
C68 C 0.08635(9) 0.3700(4) 0.92127(12) 0.074(4) Uani 1 1 d D . . . .
C69 C 0.07237(9) 0.4515(3) 0.91033(14) 0.073(4) Uani 1 1 d D . . . .
H69 H 0.0761 0.5269 0.9132 0.088 Uiso 1 1 calc R U . . .
C70 C 0.05319(9) 0.4251(3) 0.89548(15) 0.086(4) Uani 1 1 d D . . . .
H70 H 0.0442 0.4826 0.8879 0.103 Uiso 1 1 calc R U . . .
C71 C 0.10292(10) 0.3865(4) 0.94366(8) 0.061(3) Uani 1 1 d D . . . .
C72 C 0.11745(11) 0.3035(4) 0.95317(8) 0.071(4) Uani 1 1 d D . . . .
H72 H 0.12 0.2393 0.9428 0.085 Uiso 1 1 calc R U . . .
C73 C 0.12825(11) 0.3127(4) 0.97732(9) 0.059(3) Uani 1 1 d D . . . .
H73 H 0.138 0.2548 0.9834 0.071 Uiso 1 1 calc R U . . .
C74 C 0.12501(13) 0.4062(4) 0.99286(8) 0.075(4) Uani 1 1 d D . . . .
C75 C 0.11180(12) 0.4919(4) 0.98255(9) 0.072(4) Uani 1 1 d D . . . .
H75 H 0.11 0.558 0.9924 0.087 Uiso 1 1 calc R U . . .
C76 C 0.10124(12) 0.4831(4) 0.95838(9) 0.068(4) Uani 1 1 d D . . . .
H76 H 0.0927 0.5438 0.9516 0.081 Uiso 1 1 calc R U . . .
O1 O 0.10389(15) 0.2371(6) 1.02438(16) 0.058(2) Uani 1 1 d . . . . .
O2 O 0.10435(16) 0.2316(6) 1.07705(16) 0.061(2) Uani 1 1 d . . . . .
O3 O 0.1498(2) 0.5694(8) 1.0751(2) 0.090(3) Uani 1 1 d . . . . .
O4 O 0.14910(18) 0.5653(7) 1.0215(2) 0.089(3) Uani 1 1 d . . . . .
Cl1 Cl -0.18528(7) -0.2402(3) 1.09386(6) 0.0900(12) Uani 1 1 d D . . B 1
Cl2 Cl -0.18543(8) -0.2411(4) 1.01021(7) 0.1067(16) Uani 1 1 d D . . B 1
C77 C -0.19263(8) -0.2372(13) 1.06046(9) 0.104(6) Uani 1 1 d D . . B 1
C78 C -0.17819(10) -0.2473(12) 1.04361(10) 0.096(5) Uani 1 1 d D . . B 1
H78 H -0.1625 -0.259 1.0485 0.115 Uiso 1 1 calc R U . B 1
Cl3 Cl -0.22184(6) -0.2139(13) 1.05276(19) 0.303(7) Uani 1 1 d D . . B 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'
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 119.0(9) . . ?
C2 C1 C74 119.6(10) . . ?
C6 C1 C74 120.8(10) . . ?
O1 C2 C1 123.3(10) . . ?
O1 C2 C3 117.8(11) . . ?
C1 C2 C3 118.9(11) . . ?
C4 C3 C2 122.4(12) . . ?
C4 C3 O2 120.3(10) . . ?
C2 C3 O2 117.0(10) . . ?
C3 C4 C5 117.7(10) . . ?
C3 C4 C11 118.2(10) . . ?
C5 C4 C11 123.3(10) . . ?
C6 C5 O3 117.3(14) . . ?
C6 C5 C4 121.2(12) . . ?
O3 C5 C4 121.4(13) . . ?
C5 C6 O4 122.2(13) . . ?
C5 C6 C1 120.8(12) . . ?
O4 C6 C1 116.7(12) . . ?
O1 C7 H7A 109.5 . . ?
O1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O2 C8 H8A 109.5 . . ?
O2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O3 C9 H9A 109.5 . . ?
O3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O4 C10 H10A 109.5 . . ?
O4 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O4 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C16 C11 C12 117.44(19) . . ?
C16 C11 C4 117.9(5) . . ?
C12 C11 C4 122.3(5) . . ?
C13 C12 C11 121.4(2) . . ?
C13 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
C12 C13 C14 120.7(2) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 H13 119.7 . . ?
C15 C14 C13 117.7(2) . . ?
C15 C14 C17 121.6(4) . . ?
C13 C14 C17 118.7(3) . . ?
C16 C15 C14 121.4(2) . . ?
C16 C15 H15 119.3 . . ?
C14 C15 H15 119.3 . . ?
C15 C16 C11 121.0(2) . . ?
C15 C16 H16 119.5 . . ?
C11 C16 H16 119.5 . . ?
C22 C17 C18 117.4(2) . . ?
C22 C17 C14 117.7(4) . . ?
C18 C17 C14 124.2(3) . . ?
C19 C18 C17 121.4(2) . . ?
C19 C18 H18 119.3 . . ?
C17 C18 H18 119.3 . . ?
C18 C19 C20 120.7(2) . . ?
C18 C19 H19 119.7 . . ?
C20 C19 H19 119.7 . . ?
C21 C20 C19 117.73(19) . . ?
C21 C20 C23B 120.4(4) . . ?
C19 C20 C23B 120.1(4) . . ?
C21 C20 C23 116.3(5) . . ?
C19 C20 C23 125.0(4) . . ?
C22 C21 C20 121.4(2) . . ?
C22 C21 H21 119.3 . . ?
C20 C21 H21 119.3 . . ?
C21 C22 C17 121.0(2) . . ?
C21 C22 H22 119.5 . . ?
C17 C22 H22 119.5 . . ?
C28 C23 C24 117.4(2) . . ?
C28 C23 C20 122.9(5) . . ?
C24 C23 C20 117.8(6) . . ?
C25 C24 C23 121.4(2) . . ?
C25 C24 H24 119.3 . . ?
C23 C24 H24 119.3 . . ?
C24 C25 C26 120.6(2) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C27 C26 C25 117.7(2) . . ?
C27 C26 C29 115.5(7) . . ?
C25 C26 C29 123.0(6) . . ?
C28 C27 C26 121.4(2) . . ?
C28 C27 H27 119.3 . . ?
C26 C27 H27 119.3 . . ?
C27 C28 C23 121.0(2) . . ?
C27 C28 H28 119.5 . . ?
C23 C28 H28 119.5 . . ?
C28B C23B C24B 117.4(2) . . ?
C28B C23B C20 123.2(4) . . ?
C24B C23B C20 114.2(5) . . ?
C25B C24B C23B 121.4(2) . . ?
C25B C24B H24B 119.3 . . ?
C23B C24B H24B 119.3 . . ?
C24B C25B C26B 120.7(2) . . ?
C24B C25B H25B 119.7 . . ?
C26B C25B H25B 119.7 . . ?
C27B C26B C25B 117.7(2) . . ?
C27B C26B C29 123.7(4) . . ?
C25B C26B C29 116.9(4) . . ?
C28B C27B C26B 121.5(2) . . ?
C28B C27B H27B 119.3 . . ?
C26B C27B H27B 119.3 . . ?
C27B C28B C23B 121.0(2) . . ?
C27B C28B H28B 119.5 . . ?
C23B C28B H28B 119.5 . . ?
C34 C29 C30 117.42(19) . . ?
C34 C29 C26B 122.5(4) . . ?
C30 C29 C26B 117.8(4) . . ?
C34 C29 C26 122.4(3) . . ?
C30 C29 C26 119.6(3) . . ?
C31 C30 C29 121.4(2) . . ?
C31 C30 H30 119.3 . . ?
C29 C30 H30 119.3 . . ?
C30 C31 C32 120.6(2) . . ?
C30 C31 H31 119.7 . . ?
C32 C31 H31 119.7 . . ?
C33 C32 C31 117.7(2) . . ?
C33 C32 C35 123.8(3) . . ?
C31 C32 C35 117.7(3) . . ?
C34 C33 C32 121.4(2) . . ?
C34 C33 H33 119.3 . . ?
C32 C33 H33 119.3 . . ?
C33 C34 C29 121.0(2) . . ?
C33 C34 H34 119.5 . . ?
C29 C34 H34 119.5 . . ?
C40 C35 C36 117.46(19) . . ?
C40 C35 C32 117.5(3) . . ?
C36 C35 C32 123.1(4) . . ?
C37 C36 C35 121.4(2) . . ?
C37 C36 H36 119.3 . . ?
C35 C36 H36 119.3 . . ?
C36 C37 C38 120.7(2) . . ?
C36 C37 H37 119.7 . . ?
C38 C37 H37 119.7 . . ?
C39 C38 C37 117.74(19) . . ?
C39 C38 C41 120.9(3) . . ?
C37 C38 C41 120.9(4) . . ?
C40 C39 C38 121.5(2) . . ?
C40 C39 H39 119.3 . . ?
C38 C39 H39 119.3 . . ?
C39 C40 C35 121.0(2) . . ?
C39 C40 H40 119.5 . . ?
C35 C40 H40 119.5 . . ?
C46 C41 C42 117.4(2) . . ?
C46 C41 C38 118.0(4) . . ?
C42 C41 C38 122.7(3) . . ?
C43 C42 C41 121.4(2) . . ?
C43 C42 H42 119.3 . . ?
C41 C42 H42 119.3 . . ?
C42 C43 C44 120.7(2) . . ?
C42 C43 H43 119.7 . . ?
C44 C43 H43 119.7 . . ?
C45 C44 C43 117.7(2) . . ?
C45 C44 C47 121.4(4) . . ?
C43 C44 C47 119.4(4) . . ?
C46 C45 C44 121.5(2) . . ?
C46 C45 H45 119.3 . . ?
C44 C45 H45 119.3 . . ?
C45 C46 C41 121.0(2) . . ?
C45 C46 H46 119.5 . . ?
C41 C46 H46 119.5 . . ?
C52 C47 C48 117.46(19) . . ?
C52 C47 C44 121.3(3) . . ?
C48 C47 C44 118.7(4) . . ?
C49 C48 C47 121.4(2) . . ?
C49 C48 H48 119.3 . . ?
C47 C48 H48 119.3 . . ?
C48 C49 C50 120.7(2) . . ?
C48 C49 H49 119.7 . . ?
C50 C49 H49 119.7 . . ?
C51 C50 C49 117.7(2) . . ?
C51 C50 C53 123.8(3) . . ?
C49 C50 C53 117.8(3) . . ?
C52 C51 C50 121.5(2) . . ?
C52 C51 H51 119.3 . . ?
C50 C51 H51 119.3 . . ?
C51 C52 C47 121.0(2) . . ?
C51 C52 H52 119.5 . . ?
C47 C52 H52 119.5 . . ?
C58 C53 C54 117.48(19) . . ?
C58 C53 C50 118.2(3) . . ?
C54 C53 C50 122.2(4) . . ?
C55 C54 C53 121.4(2) . . ?
C55 C54 H54 119.3 . . ?
C53 C54 H54 119.3 . . ?
C54 C55 C56 120.7(2) . . ?
C54 C55 H55 119.7 . . ?
C56 C55 H55 119.7 . . ?
C57 C56 C55 117.76(19) . . ?
C57 C56 C59 124.1(4) . . ?
C55 C56 C59 114.4(4) . . ?
C58 C57 C56 121.5(2) . . ?
C58 C57 H57 119.3 . . ?
C56 C57 H57 119.3 . . ?
C57 C58 C53 121.1(2) . . ?
C57 C58 H58 119.5 . . ?
C53 C58 H58 119.5 . . ?
C64 C59 C60 117.5(2) . . ?
C64 C59 C56 121.1(4) . . ?
C60 C59 C56 121.2(4) . . ?
C61 C60 C59 121.4(2) . . ?
C61 C60 H60 119.3 . . ?
C59 C60 H60 119.3 . . ?
C60 C61 C62 120.6(2) . . ?
C60 C61 H61 119.7 . . ?
C62 C61 H61 119.7 . . ?
C63 C62 C61 117.7(2) . . ?
C63 C62 C65 125.1(4) . . ?
C61 C62 C65 115.3(4) . . ?
C64 C63 C62 121.4(2) . . ?
C64 C63 H63 119.3 . . ?
C62 C63 H63 119.3 . . ?
C63 C64 C59 121.0(2) . . ?
C63 C64 H64 119.5 . . ?
C59 C64 H64 119.5 . . ?
C70 C65 C66 117.40(19) . . ?
C70 C65 C62 120.3(4) . . ?
C66 C65 C62 119.8(4) . . ?
C67 C66 C65 121.4(2) . . ?
C67 C66 H66 119.3 . . ?
C65 C66 H66 119.3 . . ?
C66 C67 C68 120.6(2) . . ?
C66 C67 H67 119.7 . . ?
C68 C67 H67 119.7 . . ?
C69 C68 C67 117.7(2) . . ?
C69 C68 C71 125.4(4) . . ?
C67 C68 C71 115.4(4) . . ?
C70 C69 C68 121.4(2) . . ?
C70 C69 H69 119.3 . . ?
C68 C69 H69 119.3 . . ?
C69 C70 C65 121.0(2) . . ?
C69 C70 H70 119.5 . . ?
C65 C70 H70 119.5 . . ?
C76 C71 C72 117.4(2) . . ?
C76 C71 C68 118.4(4) . . ?
C72 C71 C68 123.4(3) . . ?
C73 C72 C71 121.4(2) . . ?
C73 C72 H72 119.3 . . ?
C71 C72 H72 119.3 . . ?
C72 C73 C74 120.7(2) . . ?
C72 C73 H73 119.7 . . ?
C74 C73 H73 119.7 . . ?
C75 C74 C73 117.74(19) . . ?
C75 C74 C1 118.3(6) . . ?
C73 C74 C1 120.2(5) . . ?
C76 C75 C74 121.5(2) . . ?
C76 C75 H75 119.3 . . ?
C74 C75 H75 119.3 . . ?
C75 C76 C71 121.0(2) . . ?
C75 C76 H76 119.5 . . ?
C71 C76 H76 119.5 . . ?
C2 O1 C7 117.7(10) . . ?
C8 O2 C3 110.2(10) . . ?
C9 O3 C5 120.3(13) . . ?
C10 O4 C6 126.1(13) . . ?
C78 C77 Cl1 121.5(2) . . ?
C78 C77 Cl3 121.5(2) . . ?
Cl1 C77 Cl3 116.9(5) . . ?
C77 C78 Cl2 121.5(2) . . ?
C77 C78 H78 119.2 . . ?
Cl2 C78 H78 119.2 . . ?
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 1.390(16) . ?
C1 C6 1.396(17) . ?
C1 C74 1.501(6) . ?
C2 O1 1.333(14) . ?
C2 C3 1.394(15) . ?
C3 C4 1.375(16) . ?
C3 O2 1.454(15) . ?
C4 C5 1.391(18) . ?
C4 C11 1.516(6) . ?
C5 C6 1.367(18) . ?
C5 O3 1.367(16) . ?
C6 O4 1.380(15) . ?
C7 O1 1.437(18) . ?
C7 H7A 0.98 . ?
C7 H7B 0.98 . ?
C7 H7C 0.98 . ?
C8 O2 1.452(18) . ?
C8 H8A 0.98 . ?
C8 H8B 0.98 . ?
C8 H8C 0.98 . ?
C9 O3 1.280(19) . ?
C9 H9A 0.98 . ?
C9 H9B 0.98 . ?
C9 H9C 0.98 . ?
C10 O4 1.35(2) . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C11 C16 1.393(3) . ?
C11 C12 1.396(3) . ?
C12 C13 1.383(3) . ?
C12 H12 0.95 . ?
C13 C14 1.394(3) . ?
C13 H13 0.95 . ?
C14 C15 1.391(3) . ?
C14 C17 1.512(5) . ?
C15 C16 1.377(3) . ?
C15 H15 0.95 . ?
C16 H16 0.95 . ?
C17 C22 1.393(3) . ?
C17 C18 1.396(3) . ?
C18 C19 1.383(3) . ?
C18 H18 0.95 . ?
C19 C20 1.394(3) . ?
C19 H19 0.95 . ?
C20 C21 1.391(3) . ?
C20 C23B 1.485(5) . ?
C20 C23 1.518(6) . ?
C21 C22 1.377(3) . ?
C21 H21 0.95 . ?
C22 H22 0.95 . ?
C23 C28 1.393(3) . ?
C23 C24 1.396(3) . ?
C24 C25 1.383(3) . ?
C24 H24 0.95 . ?
C25 C26 1.394(3) . ?
C25 H25 0.95 . ?
C26 C27 1.391(3) . ?
C26 C29 1.522(6) . ?
C27 C28 1.377(3) . ?
C27 H27 0.95 . ?
C28 H28 0.95 . ?
C23B C28B 1.393(3) . ?
C23B C24B 1.396(3) . ?
C24B C25B 1.383(3) . ?
C24B H24B 0.95 . ?
C25B C26B 1.394(3) . ?
C25B H25B 0.95 . ?
C26B C27B 1.391(3) . ?
C26B C29 1.487(5) . ?
C27B C28B 1.377(3) . ?
C27B H27B 0.95 . ?
C28B H28B 0.95 . ?
C29 C34 1.393(3) . ?
C29 C30 1.396(3) . ?
C30 C31 1.383(3) . ?
C30 H30 0.95 . ?
C31 C32 1.394(3) . ?
C31 H31 0.95 . ?
C32 C33 1.391(3) . ?
C32 C35 1.517(5) . ?
C33 C34 1.377(3) . ?
C33 H33 0.95 . ?
C34 H34 0.95 . ?
C35 C40 1.393(3) . ?
C35 C36 1.395(3) . ?
C36 C37 1.383(3) . ?
C36 H36 0.95 . ?
C37 C38 1.394(3) . ?
C37 H37 0.95 . ?
C38 C39 1.391(3) . ?
C38 C41 1.510(4) . ?
C39 C40 1.377(3) . ?
C39 H39 0.95 . ?
C40 H40 0.95 . ?
C41 C46 1.393(3) . ?
C41 C42 1.396(3) . ?
C42 C43 1.383(3) . ?
C42 H42 0.95 . ?
C43 C44 1.394(3) . ?
C43 H43 0.95 . ?
C44 C45 1.391(3) . ?
C44 C47 1.510(5) . ?
C45 C46 1.377(3) . ?
C45 H45 0.95 . ?
C46 H46 0.95 . ?
C47 C52 1.393(3) . ?
C47 C48 1.395(3) . ?
C48 C49 1.383(3) . ?
C48 H48 0.95 . ?
C49 C50 1.394(3) . ?
C49 H49 0.95 . ?
C50 C51 1.391(3) . ?
C50 C53 1.502(5) . ?
C51 C52 1.377(3) . ?
C51 H51 0.95 . ?
C52 H52 0.95 . ?
C53 C58 1.393(3) . ?
C53 C54 1.395(3) . ?
C54 C55 1.383(3) . ?
C54 H54 0.95 . ?
C55 C56 1.393(3) . ?
C55 H55 0.95 . ?
C56 C57 1.391(3) . ?
C56 C59 1.495(4) . ?
C57 C58 1.377(3) . ?
C57 H57 0.95 . ?
C58 H58 0.95 . ?
C59 C64 1.393(3) . ?
C59 C60 1.395(3) . ?
C60 C61 1.383(3) . ?
C60 H60 0.95 . ?
C61 C62 1.394(3) . ?
C61 H61 0.95 . ?
C62 C63 1.391(3) . ?
C62 C65 1.507(5) . ?
C63 C64 1.377(3) . ?
C63 H63 0.95 . ?
C64 H64 0.95 . ?
C65 C70 1.393(3) . ?
C65 C66 1.396(3) . ?
C66 C67 1.383(3) . ?
C66 H66 0.95 . ?
C67 C68 1.394(3) . ?
C67 H67 0.95 . ?
C68 C69 1.391(3) . ?
C68 C71 1.501(5) . ?
C69 C70 1.377(3) . ?
C69 H69 0.95 . ?
C70 H70 0.95 . ?
C71 C76 1.393(3) . ?
C71 C72 1.396(3) . ?
C72 C73 1.383(3) . ?
C72 H72 0.95 . ?
C73 C74 1.394(3) . ?
C73 H73 0.95 . ?
C74 C75 1.391(3) . ?
C75 C76 1.377(3) . ?
C75 H75 0.95 . ?
C76 H76 0.95 . ?
Cl1 C77 1.753(4) . ?
Cl2 C78 1.753(4) . ?
C77 C78 1.202(11) . ?
C77 Cl3 1.753(4) . ?
C78 H78 0.95 . ?
