# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_aak_4101_acetone_sync
_database_code_depnum_ccdc_archive 'CCDC 2264974'
loop_
_audit_author_name
_audit_author_address
'Werner Kaminsky'
;University of Washington
United States of America
;
_audit_update_record             
;
2023-05-23 deposited with the CCDC.	2023-08-17 downloaded from the CCDC.
;

_audit_creation_date             2023-04-18T14:43:42-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.5
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C84 H72 O12, 2(C3 H6 O)'
_chemical_formula_sum            'C90 H84 O14'
_chemical_formula_weight         1389.57

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   20.514(3)
_cell_length_b                   9.4966(13)
_cell_length_c                   39.416(6)
_cell_angle_alpha                90
_cell_angle_beta                 104.097(5)
_cell_angle_gamma                90
_cell_volume                     7447.4(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9311
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      26.83
_cell_measurement_wavelength     0.7288

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       shard
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2944

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.736
_exptl_absorpt_correction_T_max  0.919
_shelx_estimated_absorpt_T_min   0.983
_shelx_estimated_absorpt_T_max   0.991

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'ALS-U Lawrence Berkeley National Laboratory'
_diffrn_source_type              'ALS-U Beamline 12.2.1'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7288
_diffrn_radiation_type           synchrotron
_diffrn_radiation_probe          X-ray
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'φ or ω oscillation scans'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_number            25207
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_theta_min         2.456
_diffrn_reflns_theta_max         25.709
_diffrn_reflns_theta_full        25.709
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_reflns_Laue_measured_fraction_full 0.99
_diffrn_reflns_Laue_measured_fraction_max 0.99
_diffrn_reflns_point_group_measured_fraction_full 0.99
_diffrn_reflns_point_group_measured_fraction_max 0.99
_reflns_Friedel_coverage         0
_reflns_number_total             13026
_reflns_number_gt                10055
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_shelx_SHELXL_version_number     2014/7
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0500P)²+20.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_coef       0.0276(17)
_refine_ls_number_reflns         13026
_refine_ls_number_parameters     969
_refine_ls_number_restraints     639
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.1445
_refine_ls_R_factor_gt           0.1274
_refine_ls_wR_factor_ref         0.282
_refine_ls_wR_factor_gt          0.2752
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.067

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017 '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 0.0115 0.0064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.7216(2) 0.0107(5) 0.10407(12) 0.0741(14) Uani 1 1 d D . . . .
C2 C 0.7801(2) -0.0614(6) 0.11921(12) 0.0813(16) Uani 1 1 d D . . . .
H2 H 0.8136 -0.0719 0.1065 0.098 Uiso 1 1 calc R U . . .
C3 C 0.7910(3) -0.1184(6) 0.15237(13) 0.0848(17) Uani 1 1 d D . . . .
H3 H 0.8322 -0.165 0.1623 0.102 Uiso 1 1 calc R U . . .
C4 C 0.7421(3) -0.1079(6) 0.17128(12) 0.0812(16) Uani 1 1 d D . . . .
C5 C 0.6801(3) -0.0517(6) 0.15447(13) 0.0875(17) Uani 1 1 d D . . . .
H5 H 0.644 -0.0541 0.1657 0.105 Uiso 1 1 calc R U . . .
C6 C 0.6703(2) 0.0080(6) 0.12136(13) 0.0823(16) Uani 1 1 d D . . . .
H6 H 0.6278 0.0475 0.1104 0.099 Uiso 1 1 calc R U . . .
C7 C 0.7613(3) -0.1315(6) 0.20965(13) 0.0908(18) Uani 1 1 d D . . . .
C8 C 0.8171(3) -0.2090(6) 0.22596(13) 0.101(2) Uani 1 1 d D . . . .
H8 H 0.8354 -0.2749 0.2127 0.121 Uiso 1 1 calc R U . . .
C9 C 0.8470(3) -0.1927(7) 0.26117(14) 0.112(2) Uani 1 1 d D . . . .
H9 H 0.8856 -0.2469 0.2716 0.134 Uiso 1 1 calc R U . . .
C10 C 0.8214(3) -0.0977(6) 0.28155(12) 0.0901(18) Uani 1 1 d D . . . .
C11 C 0.7605(3) -0.0343(7) 0.26624(13) 0.102(2) Uani 1 1 d D . . . .
H11 H 0.7389 0.0224 0.2801 0.122 Uiso 1 1 calc R U . . .
C12 C 0.7304(3) -0.0526(7) 0.23080(13) 0.097(2) Uani 1 1 d D . . . .
H12 H 0.6881 -0.0101 0.221 0.116 Uiso 1 1 calc R U . . .
C13 C 0.8614(3) -0.0382(6) 0.31469(14) 0.0940(19) Uani 1 1 d D . . . .
C14 C 0.9301(3) -0.0300(7) 0.31928(17) 0.113(3) Uani 1 1 d D . . . .
H14 H 0.9511 -0.085 0.3048 0.136 Uiso 1 1 calc R U . . .
C15 C 0.9693(3) 0.0566(8) 0.34447(18) 0.119(3) Uani 1 1 d D . . . .
H15 H 1.0166 0.0592 0.3473 0.142 Uiso 1 1 calc R U . . .
C16 C 0.9397(3) 0.1397(6) 0.36570(14) 0.0848(17) Uani 1 1 d D . . . .
C17 C 0.8719(3) 0.1220(6) 0.36324(13) 0.0856(17) Uani 1 1 d D . . . .
H17 H 0.8515 0.171 0.3789 0.103 Uiso 1 1 calc R U . . .
C18 C 0.8331(3) 0.0336(6) 0.33816(14) 0.0897(18) Uani 1 1 d D . . . .
H18 H 0.7866 0.0223 0.3371 0.108 Uiso 1 1 calc R U . . .
C19 C 0.9776(3) 0.2615(5) 0.38416(11) 0.0826(16) Uani 1 1 d D . . . .
C20 C 0.9987(3) 0.2765(5) 0.42033(11) 0.0809(16) Uani 1 1 d D . . . .
C21 C 1.0365(3) 0.3901(5) 0.43570(10) 0.0793(16) Uani 1 1 d D . . . .
C22 C 1.0565(3) 0.4939(5) 0.41479(11) 0.0749(15) Uani 1 1 d D . . . .
C23 C 1.0344(3) 0.4799(5) 0.37875(11) 0.0793(16) Uani 1 1 d D . . . .
C24 C 0.9964(3) 0.3658(5) 0.36356(11) 0.0804(16) Uani 1 1 d D . . . .
O1 O 0.9846(3) 0.1696(5) 0.44098(11) 0.1088(15) Uani 1 1 d D . . . .
C25 C 0.9364(4) 0.2033(11) 0.4596(2) 0.154(4) Uani 1 1 d D . . . .
H25A H 0.9294 0.1219 0.4736 0.231 Uiso 1 1 calc R U . . .
H25B H 0.9524 0.2833 0.4751 0.231 Uiso 1 1 calc R U . . .
H25C H 0.894 0.2283 0.4431 0.231 Uiso 1 1 calc R U . . .
O2 O 1.0596(3) 0.4035(5) 0.47117(9) 0.1068(15) Uani 1 1 d D . . . .
C26 C 1.1017(4) 0.2952(8) 0.48843(19) 0.143(4) Uani 1 1 d D . . . .
H26A H 1.1152 0.3154 0.5136 0.215 Uiso 1 1 calc R U . . .
H26B H 1.0775 0.2054 0.4846 0.215 Uiso 1 1 calc R U . . .
H26C H 1.1418 0.2894 0.4792 0.215 Uiso 1 1 calc R U . . .
O3 O 1.0539(2) 0.5780(5) 0.35725(10) 0.1015(14) Uani 1 1 d D . . . .
C27 C 1.0056(4) 0.6881(8) 0.3470(2) 0.140(3) Uani 1 1 d D . . . .
H27A H 1.0216 0.7548 0.3318 0.21 Uiso 1 1 calc R U . . .
H27B H 0.9627 0.6477 0.3342 0.21 Uiso 1 1 calc R U . . .
H27C H 0.9994 0.7374 0.3678 0.21 Uiso 1 1 calc R U . . .
O4 O 0.9698(2) 0.3614(5) 0.32775(9) 0.1009(14) Uani 1 1 d D . . . .
C28 C 1.0165(4) 0.3437(12) 0.30677(19) 0.153(4) Uani 1 1 d D . . . .
H28A H 0.9925 0.3421 0.282 0.23 Uiso 1 1 calc R U . . .
H28B H 1.0486 0.4221 0.3109 0.23 Uiso 1 1 calc R U . . .
H28C H 1.0408 0.2548 0.3129 0.23 Uiso 1 1 calc R U . . .
C29 C 1.1011(2) 0.6166(5) 0.42808(13) 0.0748(15) Uani 1 1 d D . . . .
C30 C 1.1626(2) 0.6250(5) 0.41987(14) 0.0748(15) Uani 1 1 d D . . . .
H30 H 1.1817 0.5421 0.4128 0.09 Uiso 1 1 calc R U . . .
C31 C 1.1972(2) 0.7506(5) 0.42160(13) 0.0743(15) Uani 1 1 d D . . . .
H31 H 1.2399 0.7523 0.4162 0.089 Uiso 1 1 calc R U . . .
C32 C 1.1703(2) 0.8744(5) 0.43122(13) 0.0733(14) Uani 1 1 d D . . . .
C33 C 1.1121(2) 0.8637(5) 0.44302(14) 0.0786(16) Uani 1 1 d D . . . .
H33 H 1.0949 0.9448 0.452 0.094 Uiso 1 1 calc R U . . .
C34 C 1.0784(2) 0.7359(5) 0.44196(14) 0.0789(16) Uani 1 1 d D . . . .
H34 H 1.0393 0.7304 0.4508 0.095 Uiso 1 1 calc R U . . .
C35 C 1.1959(2) 1.0125(5) 0.42029(12) 0.0710(14) Uani 1 1 d D . . . .
C36 C 1.2607(2) 1.0283(5) 0.41627(12) 0.0701(14) Uani 1 1 d D . . . .
H36 H 1.2951 0.968 0.4289 0.084 Uiso 1 1 calc R U . . .
C37 C 1.2766(2) 1.1295(5) 0.39442(12) 0.0719(14) Uani 1 1 d D . . . .
H37 H 1.3213 1.1356 0.3916 0.086 Uiso 1 1 calc R U . . .
C38 C 1.2278(2) 1.2231(5) 0.37639(12) 0.0694(14) Uani 1 1 d D . . . .
C39 C 1.1661(2) 1.2215(5) 0.38485(13) 0.0782(16) Uani 1 1 d D . . . .
H39 H 1.134 1.2927 0.3758 0.094 Uiso 1 1 calc R U . . .
C40 C 1.1500(2) 1.1172(5) 0.40640(13) 0.0769(15) Uani 1 1 d D . . . .
H40 H 1.1072 1.118 0.4116 0.092 Uiso 1 1 calc R U . . .
C41 C 1.2352(2) 1.2967(4) 0.34396(11) 0.0684(14) Uani 1 1 d D . . . .
C42 C 1.2714(3) 1.2305(5) 0.32305(11) 0.0697(14) Uani 1 1 d D . . . .
H42 H 1.3001 1.1541 0.3324 0.084 Uiso 1 1 calc R U . . .
C43 C 1.2668(2) 1.2727(4) 0.28906(11) 0.0687(13) Uani 1 1 d D . . . .
H43 H 1.2917 1.224 0.2753 0.082 Uiso 1 1 calc R U . . .
C44 C 1.2262(2) 1.3858(4) 0.27466(10) 0.0652(13) Uani 1 1 d D . . . .
C45 C 1.1953(2) 1.4613(4) 0.29653(11) 0.0722(15) Uani 1 1 d D . . . .
H45 H 1.1717 1.5456 0.2883 0.087 Uiso 1 1 calc R U . . .
C46 C 1.1983(3) 1.4148(5) 0.33041(11) 0.0720(14) Uani 1 1 d D . . . .
H46 H 1.1746 1.465 0.3445 0.086 Uiso 1 1 calc R U . . .
C47 C 1.2107(2) 1.4020(5) 0.23540(11) 0.0668(13) Uani 1 1 d D . . . .
C48 C 1.2588(2) 1.3761(5) 0.21654(11) 0.0665(13) Uani 1 1 d D . . . .
C49 C 1.2411(2) 1.3419(5) 0.18127(11) 0.0688(14) Uani 1 1 d D . . . .
C50 C 1.1729(2) 1.3386(5) 0.16317(11) 0.0671(13) Uani 1 1 d D . . . .
C51 C 1.1259(2) 1.3784(5) 0.18120(11) 0.0671(13) Uani 1 1 d D . . . .
C52 C 1.1436(2) 1.4109(5) 0.21654(11) 0.0683(13) Uani 1 1 d D . . . .
O5 O 1.32585(16) 1.3680(4) 0.23336(9) 0.0759(10) Uani 1 1 d D . . . .
C53 C 1.3544(3) 1.4928(7) 0.2502(2) 0.115(3) Uani 1 1 d D . . . .
H53A H 1.402 1.4767 0.2614 0.172 Uiso 1 1 calc R U . . .
H53B H 1.3503 1.5686 0.233 0.172 Uiso 1 1 calc R U . . .
H53C H 1.3306 1.5195 0.268 0.172 Uiso 1 1 calc R U . . .
O6 O 1.28782(17) 1.3016(4) 0.16359(9) 0.0772(10) Uani 1 1 d D U . . .
C54 C 1.3432(3) 1.3905(8) 0.16523(19) 0.114(2) Uani 1 1 d D U . . .
H54A H 1.3724 1.3495 0.1515 0.171 Uiso 1 1 calc R U . . .
H54B H 1.3274 1.483 0.1556 0.171 Uiso 1 1 calc R U . . .
H54C H 1.3684 1.4009 0.1896 0.171 Uiso 1 1 calc R U . . .
O7 O 1.05857(16) 1.3804(4) 0.16391(10) 0.0827(11) Uani 1 1 d D U . . .
C55 C 1.0245(4) 1.2532(8) 0.1687(2) 0.136(3) Uani 1 1 d D U . . .
H55A H 0.9772 1.2599 0.156 0.204 Uiso 1 1 calc R U . . .
H55B H 1.0455 1.1734 0.1597 0.204 Uiso 1 1 calc R U . . .
H55C H 1.0275 1.2393 0.1936 0.204 Uiso 1 1 calc R U . . .
O8 O 1.09317(18) 1.4312(4) 0.23381(9) 0.0818(11) Uani 1 1 d D U . . .
C56 C 1.0596(4) 1.5636(7) 0.2287(2) 0.125(3) Uani 1 1 d D U . . .
H56A H 1.0251 1.5662 0.2421 0.187 Uiso 1 1 calc R U . . .
H56B H 1.0922 1.6393 0.2367 0.187 Uiso 1 1 calc R U . . .
H56C H 1.0384 1.5764 0.2038 0.187 Uiso 1 1 calc R U . . .
C57 C 1.1509(2) 1.2636(4) 0.12876(11) 0.0689(13) Uani 1 1 d D . . . .
C58 C 1.1722(2) 1.1257(5) 0.12755(12) 0.0706(14) Uani 1 1 d D . . . .
H58 H 1.209 1.0926 0.1453 0.085 Uiso 1 1 calc R U . . .
C59 C 1.1412(2) 1.0353(5) 0.10111(12) 0.0745(15) Uani 1 1 d D . . . .
H59 H 1.1568 0.9412 0.1011 0.089 Uiso 1 1 calc R U . . .
C60 C 1.0873(2) 1.0799(5) 0.07452(11) 0.0680(13) Uani 1 1 d D . . . .
C61 C 1.0706(3) 1.2216(5) 0.07370(12) 0.0768(15) Uani 1 1 d D . . . .
H61 H 1.0376 1.2577 0.0544 0.092 Uiso 1 1 calc R U . . .
C62 C 1.1012(2) 1.3118(4) 0.10070(12) 0.0736(15) Uani 1 1 d D . . . .
H62 H 1.0879 1.4078 0.0999 0.088 Uiso 1 1 calc R U . . .
C63 C 1.0436(2) 0.9724(5) 0.05225(12) 0.0695(14) Uani 1 1 d D . . . .
C64 C 1.0678(2) 0.8433(5) 0.04459(14) 0.0760(15) Uani 1 1 d D . . . .
H64 H 1.1149 0.8297 0.0486 0.091 Uiso 1 1 calc R U . . .
C65 C 1.0249(2) 0.7335(5) 0.03129(13) 0.0776(15) Uani 1 1 d D . . . .
H65 H 1.043 0.6463 0.0261 0.093 Uiso 1 1 calc R U . . .
C66 C 0.9556(2) 0.7489(5) 0.02538(12) 0.0696(14) Uani 1 1 d D . . . .
C67 C 0.9312(2) 0.8818(5) 0.02969(13) 0.0750(15) Uani 1 1 d D . . . .
H67 H 0.884 0.898 0.0236 0.09 Uiso 1 1 calc R U . . .
C68 C 0.9747(2) 0.9922(5) 0.04279(14) 0.0762(15) Uani 1 1 d D . . . .
H68 H 0.9567 1.0828 0.0453 0.091 Uiso 1 1 calc R U . . .
C69 C 0.9096(2) 0.6265(5) 0.01932(12) 0.0717(14) Uani 1 1 d D . . . .
C70 C 0.9316(2) 0.4982(5) 0.03429(14) 0.0803(16) Uani 1 1 d D . . . .
H70 H 0.9784 0.4836 0.0436 0.096 Uiso 1 1 calc R U . . .
C71 C 0.8871(2) 0.3905(5) 0.03606(15) 0.0838(17) Uani 1 1 d D . . . .
H71 H 0.9038 0.303 0.0463 0.101 Uiso 1 1 calc R U . . .
C72 C 0.8183(2) 0.4088(5) 0.02308(13) 0.0737(15) Uani 1 1 d D . . . .
C73 C 0.7963(2) 0.5337(5) 0.00585(13) 0.0771(15) Uani 1 1 d D . . . .
H73 H 0.7498 0.547 -0.0044 0.093 Uiso 1 1 calc R U . . .
C74 C 0.8418(2) 0.6398(5) 0.00348(13) 0.0783(16) Uani 1 1 d D . . . .
H74 H 0.826 0.723 -0.0093 0.094 Uiso 1 1 calc R U . . .
C75 C 0.7741(3) 0.3045(4) 0.03430(13) 0.0744(15) Uani 1 1 d D . . . .
C76 C 0.7795(3) 0.1607(4) 0.02862(13) 0.0760(15) Uani 1 1 d D . . . .
C77 C 0.7548(3) 0.0620(4) 0.04808(13) 0.0743(15) Uani 1 1 d D . . . .
C78 C 0.7242(3) 0.1050(4) 0.07468(12) 0.0721(14) Uani 1 1 d D . . . .
C79 C 0.7108(3) 0.2480(4) 0.07694(12) 0.0703(14) Uani 1 1 d D . . . .
C80 C 0.7344(3) 0.3456(4) 0.05670(13) 0.0720(14) Uani 1 1 d D . . . .
O9 O 0.8130(2) 0.1130(4) 0.00452(10) 0.0925(13) Uani 1 1 d D . . . .
C81 C 0.7729(4) 0.0962(10) -0.02953(15) 0.130(3) Uani 1 1 d D . . . .
H81A H 0.8006 0.0621 -0.0448 0.195 Uiso 1 1 calc R U . . .
H81B H 0.7372 0.0278 -0.0293 0.195 Uiso 1 1 calc R U . . .
H81C H 0.7528 0.1869 -0.0382 0.195 Uiso 1 1 calc R U . . .
O10 O 0.7636(2) -0.0792(3) 0.04270(11) 0.0886(12) Uani 1 1 d D . . . .
C82 C 0.7057(4) -0.1532(7) 0.0260(3) 0.136(3) Uani 1 1 d D . . . .
H82A H 0.7172 -0.2522 0.0234 0.203 Uiso 1 1 calc R U . . .
H82B H 0.6725 -0.1472 0.0401 0.203 Uiso 1 1 calc R U . . .
H82C H 0.687 -0.1122 0.0029 0.203 Uiso 1 1 calc R U . . .
O11 O 0.67870(19) 0.2964(4) 0.10163(9) 0.0763(10) Uani 1 1 d D . . . .
C83 C 0.6088(3) 0.3254(7) 0.08709(18) 0.099(2) Uani 1 1 d D . . . .
H83A H 0.5883 0.3594 0.1056 0.149 Uiso 1 1 calc R U . . .
H83B H 0.6043 0.3976 0.0689 0.149 Uiso 1 1 calc R U . . .
H83C H 0.586 0.2391 0.0769 0.149 Uiso 1 1 calc R U . . .
O12 O 0.7225(2) 0.4878(3) 0.06110(10) 0.0842(11) Uani 1 1 d D . . . .
C84 C 0.7698(4) 0.5518(7) 0.08948(16) 0.102(2) Uani 1 1 d D . . . .
H84A H 0.7584 0.6514 0.091 0.153 Uiso 1 1 calc R U . . .
H84B H 0.7684 0.504 0.1113 0.153 Uiso 1 1 calc R U . . .
H84C H 0.815 0.5439 0.0856 0.153 Uiso 1 1 calc R U . . .
O13 O 0.8944(5) 0.4161(10) 0.2135(3) 0.244(5) Uani 1 1 d D . . . .
C85 C 0.8235(7) 0.2671(14) 0.1738(3) 0.206(6) Uani 1 1 d D . . . .
H85A H 0.8087 0.169 0.1739 0.308 Uiso 1 1 calc R U . . .
H85B H 0.7844 0.3295 0.1699 0.308 Uiso 1 1 calc R U . . .
H85C H 0.8466 0.2804 0.155 0.308 Uiso 1 1 calc R U . . .
C86 C 0.8701(6) 0.3008(14) 0.2079(3) 0.166(4) Uani 1 1 d D . . . .
C87 C 0.8807(8) 0.1759(14) 0.2310(4) 0.243(8) Uani 1 1 d D . . . .
H87A H 0.8537 0.0973 0.219 0.365 Uiso 1 1 calc R U . . .
H87B H 0.9283 0.1498 0.2367 0.365 Uiso 1 1 calc R U . . .
H87C H 0.867 0.1978 0.2526 0.365 Uiso 1 1 calc R U . . .
O14 O 0.9694(5) -0.1464(13) 0.1711(3) 0.199(4) Uani 0.784(8) 1 d D U P A 1
C88 C 0.9386(8) -0.3261(18) 0.1291(5) 0.208(6) Uani 0.784(8) 1 d D U P A 1
H88A H 0.959 -0.3694 0.1116 0.312 Uiso 0.784(8) 1 calc R U P A 1
H88B H 0.9316 -0.3981 0.1456 0.312 Uiso 0.784(8) 1 calc R U P A 1
H88C H 0.8953 -0.2842 0.1174 0.312 Uiso 0.784(8) 1 calc R U P A 1
C89 C 0.9838(9) -0.215(2) 0.1481(5) 0.189(4) Uani 0.784(8) 1 d D U P A 1
C90 C 1.0484(8) -0.227(2) 0.1376(5) 0.199(5) Uani 0.784(8) 1 d D U P A 1
H90A H 1.0429 -0.2921 0.1179 0.299 Uiso 0.784(8) 1 calc R U P A 1
H90B H 1.0616 -0.1342 0.1308 0.299 Uiso 0.784(8) 1 calc R U P A 1
H90C H 1.0832 -0.2628 0.1574 0.299 Uiso 0.784(8) 1 calc R U P A 1
O14B O 0.9869(19) 0.005(4) 0.1447(11) 0.209(8) Uani 0.216(8) 1 d D U P A 2
C88B C 1.072(2) -0.148(6) 0.1748(13) 0.202(8) Uani 0.216(8) 1 d D U P A 2
H88D H 1.0892 -0.2409 0.1704 0.303 Uiso 0.216(8) 1 calc R U P A 2
H88E H 1.1087 -0.0783 0.1771 0.303 Uiso 0.216(8) 1 calc R U P A 2
H88F H 1.0569 -0.1499 0.1964 0.303 Uiso 0.216(8) 1 calc R U P A 2
C89B C 1.016(3) -0.108(5) 0.1451(14) 0.189(4) Uani 0.216(8) 1 d D U P A 2
C90B C 0.999(3) -0.228(6) 0.1201(15) 0.195(7) Uani 0.216(8) 1 d D U P A 2
H90D H 1.0323 -0.3035 0.1275 0.292 Uiso 0.216(8) 1 calc R U P A 2
H90E H 0.9543 -0.2631 0.1198 0.292 Uiso 0.216(8) 1 calc R U P A 2
H90F H 1.0006 -0.1961 0.0966 0.292 Uiso 0.216(8) 1 calc R U P A 2



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 1.384(4) . ?
C1 C6 1.386(4) . ?
C1 C78 1.475(6) . ?
C2 C3 1.382(4) . ?
C2 H2 0.95 . ?
C3 C4 1.392(4) . ?
C3 H3 0.95 . ?
C4 C5 1.390(4) . ?
C4 C7 1.484(7) . ?
C5 C6 1.392(4) . ?
C5 H5 0.95 . ?
C6 H6 0.95 . ?
C7 C8 1.381(4) . ?
C7 C12 1.383(4) . ?
C8 C9 1.383(4) . ?
C8 H8 0.95 . ?
C9 C10 1.393(4) . ?
C9 H9 0.95 . ?
C10 C11 1.386(4) . ?
C10 C13 1.475(7) . ?
C11 C12 1.394(4) . ?
C11 H11 0.95 . ?
C12 H12 0.95 . ?
C13 C14 1.380(4) . ?
C13 C18 1.386(4) . ?
C14 C15 1.385(4) . ?
C14 H14 0.95 . ?
C15 C16 1.393(4) . ?
C15 H15 0.95 . ?
C16 C17 1.381(4) . ?
C16 C19 1.481(7) . ?
C17 C18 1.390(4) . ?
C17 H17 0.95 . ?
C18 H18 0.95 . ?
C19 C20 1.392(5) . ?
C19 C24 1.394(5) . ?
C20 O1 1.376(4) . ?
C20 C21 1.380(5) . ?
C21 O2 1.368(4) . ?
C21 C22 1.408(5) . ?
C22 C23 1.389(5) . ?
C22 C29 1.495(6) . ?
C23 O3 1.383(4) . ?
C23 C24 1.383(5) . ?
C24 O4 1.384(4) . ?
O1 C25 1.403(6) . ?
C25 H25A 0.98 . ?
C25 H25B 0.98 . ?
C25 H25C 0.98 . ?
O2 C26 1.408(6) . ?
C26 H26A 0.98 . ?
C26 H26B 0.98 . ?
C26 H26C 0.98 . ?
O3 C27 1.430(6) . ?
C27 H27A 0.98 . ?
C27 H27B 0.98 . ?
C27 H27C 0.98 . ?
O4 C28 1.421(6) . ?
C28 H28A 0.98 . ?
C28 H28B 0.98 . ?
C28 H28C 0.98 . ?
C29 C30 1.380(4) . ?
C29 C34 1.387(4) . ?
C30 C31 1.381(4) . ?
C30 H30 0.95 . ?
C31 C32 1.391(4) . ?
C31 H31 0.95 . ?
C32 C33 1.388(4) . ?
C32 C35 1.514(6) . ?
C33 C34 1.392(4) . ?
C33 H33 0.95 . ?
C34 H34 0.95 . ?
C35 C36 1.384(4) . ?
C35 C40 1.387(4) . ?
C36 C37 1.382(4) . ?
C36 H36 0.95 . ?
C37 C38 1.396(4) . ?
C37 H37 0.95 . ?
C38 C39 1.387(4) . ?
C38 C41 1.497(6) . ?
C39 C40 1.395(4) . ?
C39 H39 0.95 . ?
C40 H40 0.95 . ?
C41 C46 1.385(4) . ?
C41 C42 1.387(4) . ?
C42 C43 1.380(4) . ?
C42 H42 0.95 . ?
C43 C44 1.392(4) . ?
C43 H43 0.95 . ?
C44 C45 1.388(4) . ?
C44 C47 1.510(6) . ?
C45 C46 1.393(4) . ?
C45 H45 0.95 . ?
C46 H46 0.95 . ?
C47 C48 1.393(5) . ?
C47 C52 1.400(5) . ?
C48 O5 1.377(4) . ?
C48 C49 1.387(5) . ?
C49 O6 1.369(4) . ?
C49 C50 1.408(5) . ?
C50 C51 1.383(5) . ?
C50 C57 1.501(6) . ?
C51 O7 1.383(4) . ?
C51 C52 1.386(5) . ?
C52 O8 1.383(4) . ?
O5 C53 1.414(5) . ?
C53 H53A 0.98 . ?
C53 H53B 0.98 . ?
C53 H53C 0.98 . ?
O6 C54 1.403(5) . ?
C54 H54A 0.98 . ?
C54 H54B 0.98 . ?
C54 H54C 0.98 . ?
O7 C55 1.431(6) . ?
C55 H55A 0.98 . ?
C55 H55B 0.98 . ?
C55 H55C 0.98 . ?
O8 C56 1.424(5) . ?
C56 H56A 0.98 . ?
C56 H56B 0.98 . ?
C56 H56C 0.98 . ?
C57 C58 1.385(4) . ?
C57 C62 1.387(4) . ?
C58 C59 1.380(4) . ?
C58 H58 0.95 . ?
C59 C60 1.391(4) . ?
C59 H59 0.95 . ?
C60 C61 1.387(4) . ?
C60 C63 1.495(6) . ?
C61 C62 1.391(4) . ?
C61 H61 0.95 . ?
C62 H62 0.95 . ?
C63 C64 1.383(4) . ?
C63 C68 1.385(4) . ?
C64 C65 1.382(4) . ?
C64 H64 0.95 . ?
C65 C66 1.390(4) . ?
C65 H65 0.95 . ?
C66 C67 1.384(4) . ?
C66 C69 1.480(6) . ?
C67 C68 1.392(4) . ?
C67 H67 0.95 . ?
C68 H68 0.95 . ?
C69 C70 1.381(4) . ?
C69 C74 1.385(4) . ?
C70 C71 1.384(4) . ?
C70 H70 0.95 . ?
C71 C72 1.390(4) . ?
C71 H71 0.95 . ?
C72 C73 1.387(4) . ?
C72 C75 1.482(6) . ?
C73 C74 1.391(4) . ?
C73 H73 0.95 . ?
C74 H74 0.95 . ?
C75 C76 1.393(5) . ?
C75 C80 1.394(5) . ?
C76 O9 1.378(4) . ?
C76 C77 1.383(5) . ?
C77 O10 1.377(4) . ?
C77 C78 1.407(5) . ?
C78 C79 1.392(5) . ?
C79 O11 1.380(4) . ?
C79 C80 1.386(5) . ?
C80 O12 1.390(4) . ?
O9 C81 1.402(5) . ?
C81 H81A 0.98 . ?
C81 H81B 0.98 . ?
C81 H81C 0.98 . ?
O10 C82 1.398(5) . ?
C82 H82A 0.98 . ?
C82 H82B 0.98 . ?
C82 H82C 0.98 . ?
O11 C83 1.436(5) . ?
C83 H83A 0.98 . ?
C83 H83B 0.98 . ?
C83 H83C 0.98 . ?
O12 C84 1.425(5) . ?
C84 H84A 0.98 . ?
C84 H84B 0.98 . ?
C84 H84C 0.98 . ?
O13 C86 1.201(12) . ?
C85 C86 1.482(13) . ?
C85 H85A 0.98 . ?
C85 H85B 0.98 . ?
C85 H85C 0.98 . ?
C86 C87 1.478(14) . ?
C87 H87A 0.98 . ?
C87 H87B 0.98 . ?
C87 H87C 0.98 . ?
O14 C89 1.210(15) . ?
C88 C89 1.483(17) . ?
C88 H88A 0.98 . ?
C88 H88B 0.98 . ?
C88 H88C 0.98 . ?
C89 C90 1.484(16) . ?
C90 H90A 0.98 . ?
C90 H90B 0.98 . ?
C90 H90C 0.98 . ?
O14B C89B 1.225(19) . ?
C88B C89B 1.48(2) . ?
C88B H88D 0.98 . ?
C88B H88E 0.98 . ?
C88B H88F 0.98 . ?
C89B C90B 1.49(2) . ?
C90B H90D 0.98 . ?
C90B H90E 0.98 . ?
C90B H90F 0.98 . ?

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 117.5(4) . . ?
C2 C1 C78 116.5(4) . . ?
C6 C1 C78 125.0(4) . . ?
C3 C2 C1 121.7(4) . . ?
C3 C2 H2 119.1 . . ?
C1 C2 H2 119.1 . . ?
C2 C3 C4 120.4(4) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C5 C4 C3 117.9(4) . . ?
C5 C4 C7 121.9(4) . . ?
C3 C4 C7 119.2(4) . . ?
C4 C5 C6 120.7(4) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C1 C6 C5 121.0(4) . . ?
C1 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
C8 C7 C12 117.2(4) . . ?
C8 C7 C4 122.6(5) . . ?
C12 C7 C4 119.1(4) . . ?
C7 C8 C9 121.5(4) . . ?
C7 C8 H8 119.3 . . ?
C9 C8 H8 119.3 . . ?
C8 C9 C10 120.9(4) . . ?
C8 C9 H9 119.5 . . ?
C10 C9 H9 119.5 . . ?
C11 C10 C9 117.2(4) . . ?
C11 C10 C13 117.8(5) . . ?
C9 C10 C13 123.5(5) . . ?
C10 C11 C12 120.9(4) . . ?
C10 C11 H11 119.5 . . ?
C12 C11 H11 119.5 . . ?
C7 C12 C11 121.1(4) . . ?
C7 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C14 C13 C18 117.7(4) . . ?
C14 C13 C10 117.9(5) . . ?
C18 C13 C10 123.1(5) . . ?
C13 C14 C15 121.6(4) . . ?
C13 C14 H14 119.2 . . ?
C15 C14 H14 119.2 . . ?
C14 C15 C16 120.3(4) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C17 C16 C15 117.9(4) . . ?
C17 C16 C19 121.9(5) . . ?
C15 C16 C19 119.0(5) . . ?
C16 C17 C18 121.1(4) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
C13 C18 C17 120.7(4) . . ?
C13 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C20 C19 C24 117.5(4) . . ?
C20 C19 C16 125.3(4) . . ?
C24 C19 C16 117.1(4) . . ?
O1 C20 C21 119.6(4) . . ?
O1 C20 C19 118.1(4) . . ?
C21 C20 C19 122.1(4) . . ?
O2 C21 C20 122.6(4) . . ?
O2 C21 C22 117.1(4) . . ?
C20 C21 C22 120.2(4) . . ?
C23 C22 C21 117.5(4) . . ?
C23 C22 C29 116.9(4) . . ?
C21 C22 C29 125.5(4) . . ?
O3 C23 C24 118.7(4) . . ?
O3 C23 C22 119.4(4) . . ?
C24 C23 C22 121.8(4) . . ?
C23 C24 O4 120.4(4) . . ?
C23 C24 C19 120.8(4) . . ?
O4 C24 C19 118.5(4) . . ?
C20 O1 C25 114.7(5) . . ?
O1 C25 H25A 109.5 . . ?
O1 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O1 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C21 O2 C26 116.4(5) . . ?
O2 C26 H26A 109.5 . . ?
O2 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
O2 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C23 O3 C27 112.5(5) . . ?
O3 C27 H27A 109.5 . . ?
O3 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
O3 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C24 O4 C28 116.3(5) . . ?
O4 C28 H28A 109.5 . . ?
O4 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
O4 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 C34 117.4(4) . . ?
C30 C29 C22 118.7(4) . . ?
C34 C29 C22 122.6(4) . . ?
C29 C30 C31 121.8(4) . . ?
C29 C30 H30 119.1 . . ?
C31 C30 H30 119.1 . . ?
C30 C31 C32 120.7(4) . . ?
C30 C31 H31 119.7 . . ?
C32 C31 H31 119.7 . . ?
C33 C32 C31 117.4(4) . . ?
C33 C32 C35 123.1(4) . . ?
C31 C32 C35 117.8(4) . . ?
C32 C33 C34 121.1(4) . . ?
C32 C33 H33 119.5 . . ?
C34 C33 H33 119.5 . . ?
C29 C34 C33 120.8(4) . . ?
C29 C34 H34 119.6 . . ?
C33 C34 H34 119.6 . . ?
C36 C35 C40 117.1(4) . . ?
C36 C35 C32 122.4(4) . . ?
C40 C35 C32 118.9(4) . . ?
C37 C36 C35 121.7(4) . . ?
C37 C36 H36 119.1 . . ?
C35 C36 H36 119.1 . . ?
C36 C37 C38 120.7(4) . . ?
C36 C37 H37 119.7 . . ?
C38 C37 H37 119.7 . . ?
C39 C38 C37 117.0(4) . . ?
C39 C38 C41 119.9(4) . . ?
C37 C38 C41 121.5(4) . . ?
C38 C39 C40 121.3(4) . . ?
C38 C39 H39 119.4 . . ?
C40 C39 H39 119.4 . . ?
C35 C40 C39 120.7(4) . . ?
C35 C40 H40 119.6 . . ?
C39 C40 H40 119.6 . . ?
C46 C41 C42 117.3(4) . . ?
C46 C41 C38 123.2(4) . . ?
C42 C41 C38 118.4(4) . . ?
C43 C42 C41 121.7(4) . . ?
C43 C42 H42 119.1 . . ?
C41 C42 H42 119.1 . . ?
C42 C43 C44 120.8(4) . . ?
C42 C43 H43 119.6 . . ?
C44 C43 H43 119.6 . . ?
C45 C44 C43 117.6(3) . . ?
C45 C44 C47 124.7(4) . . ?
C43 C44 C47 116.9(4) . . ?
C44 C45 C46 120.7(3) . . ?
C44 C45 H45 119.6 . . ?
C46 C45 H45 119.6 . . ?
C41 C46 C45 121.2(4) . . ?
C41 C46 H46 119.4 . . ?
C45 C46 H46 119.4 . . ?
C48 C47 C52 117.4(4) . . ?
C48 C47 C44 122.0(4) . . ?
C52 C47 C44 119.0(4) . . ?
O5 C48 C49 117.1(4) . . ?
O5 C48 C47 120.4(4) . . ?
C49 C48 C47 122.0(4) . . ?
O6 C49 C48 122.1(4) . . ?
O6 C49 C50 117.9(4) . . ?
C48 C49 C50 119.8(4) . . ?
C51 C50 C49 117.7(4) . . ?
C51 C50 C57 120.0(4) . . ?
C49 C50 C57 120.8(4) . . ?
C50 C51 O7 119.2(4) . . ?
C50 C51 C52 122.2(4) . . ?
O7 C51 C52 118.5(4) . . ?
O8 C52 C51 118.8(4) . . ?
O8 C52 C47 120.3(4) . . ?
C51 C52 C47 120.2(4) . . ?
C48 O5 C53 115.5(4) . . ?
O5 C53 H53A 109.5 . . ?
O5 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
O5 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C49 O6 C54 117.8(4) . . ?
O6 C54 H54A 109.5 . . ?
O6 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
O6 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C51 O7 C55 112.6(4) . . ?
O7 C55 H55A 109.5 . . ?
O7 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
O7 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C52 O8 C56 116.5(5) . . ?
O8 C56 H56A 109.5 . . ?
O8 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
O8 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C58 C57 C62 117.5(3) . . ?
C58 C57 C50 116.9(4) . . ?
C62 C57 C50 124.4(4) . . ?
C59 C58 C57 121.5(4) . . ?
C59 C58 H58 119.2 . . ?
C57 C58 H58 119.2 . . ?
C58 C59 C60 121.0(4) . . ?
C58 C59 H59 119.5 . . ?
C60 C59 H59 119.5 . . ?
C61 C60 C59 117.4(4) . . ?
C61 C60 C63 122.7(4) . . ?
C59 C60 C63 119.2(4) . . ?
C60 C61 C62 121.1(4) . . ?
C60 C61 H61 119.5 . . ?
C62 C61 H61 119.5 . . ?
C57 C62 C61 121.0(4) . . ?
C57 C62 H62 119.5 . . ?
C61 C62 H62 119.5 . . ?
C64 C63 C68 117.3(4) . . ?
C64 C63 C60 122.6(4) . . ?
C68 C63 C60 119.5(4) . . ?
C65 C64 C63 121.5(4) . . ?
C65 C64 H64 119.3 . . ?
C63 C64 H64 119.3 . . ?
C64 C65 C66 120.9(4) . . ?
C64 C65 H65 119.5 . . ?
C66 C65 H65 119.5 . . ?
C67 C66 C65 117.5(4) . . ?
C67 C66 C69 120.0(4) . . ?
C65 C66 C69 122.0(4) . . ?
C66 C67 C68 120.9(4) . . ?
C66 C67 H67 119.6 . . ?
C68 C67 H67 119.6 . . ?
C63 C68 C67 121.2(4) . . ?
C63 C68 H68 119.4 . . ?
C67 C68 H68 119.4 . . ?
C70 C69 C74 117.5(4) . . ?
C70 C69 C66 119.6(4) . . ?
C74 C69 C66 122.2(4) . . ?
C69 C70 C71 121.5(4) . . ?
C69 C70 H70 119.2 . . ?
C71 C70 H70 119.2 . . ?
C70 C71 C72 120.8(4) . . ?
C70 C71 H71 119.6 . . ?
C72 C71 H71 119.6 . . ?
C73 C72 C71 117.9(4) . . ?
C73 C72 C75 124.6(4) . . ?
C71 C72 C75 116.6(4) . . ?
C72 C73 C74 120.5(4) . . ?
C72 C73 H73 119.7 . . ?
C74 C73 H73 119.7 . . ?
C69 C74 C73 121.4(4) . . ?
C69 C74 H74 119.3 . . ?
C73 C74 H74 119.3 . . ?
C76 C75 C80 117.3(4) . . ?
C76 C75 C72 121.9(4) . . ?
C80 C75 C72 119.8(4) . . ?
O9 C76 C77 118.1(4) . . ?
O9 C76 C75 120.4(4) . . ?
C77 C76 C75 121.4(4) . . ?
O10 C77 C76 119.6(4) . . ?
O10 C77 C78 119.8(4) . . ?
C76 C77 C78 120.5(4) . . ?
C79 C78 C77 117.5(4) . . ?
C79 C78 C1 119.8(4) . . ?
C77 C78 C1 121.1(4) . . ?
O11 C79 C80 118.5(4) . . ?
O11 C79 C78 120.4(4) . . ?
C80 C79 C78 120.9(4) . . ?
C79 C80 O12 118.8(4) . . ?
C79 C80 C75 121.2(4) . . ?
O12 C80 C75 119.9(4) . . ?
C76 O9 C81 115.0(5) . . ?
O9 C81 H81A 109.5 . . ?
O9 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
O9 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
C77 O10 C82 115.7(4) . . ?
O10 C82 H82A 109.5 . . ?
O10 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
O10 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C79 O11 C83 112.6(4) . . ?
O11 C83 H83A 109.5 . . ?
O11 C83 H83B 109.5 . . ?
H83A C83 H83B 109.5 . . ?
O11 C83 H83C 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?
C80 O12 C84 113.9(4) . . ?
O12 C84 H84A 109.5 . . ?
O12 C84 H84B 109.5 . . ?
H84A C84 H84B 109.5 . . ?
O12 C84 H84C 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
C86 C85 H85A 109.5 . . ?
C86 C85 H85B 109.5 . . ?
H85A C85 H85B 109.5 . . ?
C86 C85 H85C 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
O13 C86 C87 128.8(13) . . ?
O13 C86 C85 120.7(13) . . ?
C87 C86 C85 110.5(11) . . ?
C86 C87 H87A 109.5 . . ?
C86 C87 H87B 109.5 . . ?
H87A C87 H87B 109.5 . . ?
C86 C87 H87C 109.5 . . ?
H87A C87 H87C 109.5 . . ?
H87B C87 H87C 109.5 . . ?
C89 C88 H88A 109.5 . . ?
C89 C88 H88B 109.5 . . ?
H88A C88 H88B 109.5 . . ?
C89 C88 H88C 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
O14 C89 C88 121.8(16) . . ?
O14 C89 C90 130.3(18) . . ?
C88 C89 C90 107.1(15) . . ?
C89 C90 H90A 109.5 . . ?
C89 C90 H90B 109.5 . . ?
H90A C90 H90B 109.5 . . ?
C89 C90 H90C 109.5 . . ?
H90A C90 H90C 109.5 . . ?
H90B C90 H90C 109.5 . . ?
C89B C88B H88D 109.5 . . ?
C89B C88B H88E 109.5 . . ?
H88D C88B H88E 109.5 . . ?
C89B C88B H88F 109.5 . . ?
H88D C88B H88F 109.5 . . ?
H88E C88B H88F 109.5 . . ?
O14B C89B C88B 121(3) . . ?
O14B C89B C90B 129(3) . . ?
C88B C89B C90B 110(2) . . ?
C89B C90B H90D 109.5 . . ?
C89B C90B H90E 109.5 . . ?
H90D C90B H90E 109.5 . . ?
C89B C90B H90F 109.5 . . ?
H90D C90B H90F 109.5 . . ?
H90E C90B H90F 109.5 . . ?


#----------------------------------------------------------------------------#
#                   SQUEEZE DETAILS                                          #
#----------------------------------------------------------------------------#


# END of CIF

_chemical_name_common            dodecamethoxy[12]cycloparaphenylene
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetone/MeOH'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_AAK_4176
_database_code_depnum_ccdc_archive 'CCDC 2264975'
loop_
_audit_author_name
_audit_author_address
'Werner Kaminsky'
;University of Washington
United States of America
;
_audit_update_record             
;
2023-05-23 deposited with the CCDC.	2023-08-17 downloaded from the CCDC.
;

_audit_creation_date             2022-06-15T14:19:03-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.5
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C38 H38 Cl2 O4 Ru2'
_chemical_formula_sum            'C38 H38 Cl2 O4 Ru2'
_chemical_formula_weight         831.72

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.6451(7)
_cell_length_b                   10.9012(6)
_cell_length_c                   14.0135(7)
_cell_angle_alpha                90
_cell_angle_beta                 109.990(3)
_cell_angle_gamma                90
_cell_volume                     1671.77(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6607
_cell_measurement_theta_min      2.72
_cell_measurement_theta_max      27.56
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       shard
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             840

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        SADABS-2012/1 - Bruker AXS area detector scaling and absorption correcti
;
_exptl_absorpt_correction_T_min  0.704
_exptl_absorpt_correction_T_max  0.736
_shelx_estimated_absorpt_T_min   0.907
_shelx_estimated_absorpt_T_max   0.947

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'sealed x-ray tube'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'APEX-II CCD'
_diffrn_orient_matrix_ub_11      -0.047037
_diffrn_orient_matrix_ub_12      -0.062342
_diffrn_orient_matrix_ub_13      0.023935
_diffrn_orient_matrix_ub_21      -0.074757
_diffrn_orient_matrix_ub_22      0.052441
_diffrn_orient_matrix_ub_23      -0.02569
_diffrn_orient_matrix_ub_31      -0.023427
_diffrn_orient_matrix_ub_32      -0.042171
_diffrn_orient_matrix_ub_33      -0.067329
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       'φ or ω oscillation scans'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0744
_diffrn_reflns_av_unetI/netI     0.053
_diffrn_reflns_number            16214
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.972
_diffrn_reflns_theta_max         28.357
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.999
_reflns_Friedel_coverage         0
_reflns_number_total             4178
_reflns_number_gt                3213
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2 software'
_computing_cell_refinement       'SAINT V8.34A integration software'
_computing_data_reduction        'SORTAV (Blessing, 1995)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_shelx_SHELXL_version_number     2014/7
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0178P)²+1.7897P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4178
_refine_ls_number_parameters     211
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0307
_refine_ls_wR_factor_ref         0.0653
_refine_ls_wR_factor_gt          0.0582
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.576
_refine_diff_density_min         -0.972
_refine_diff_density_rms         0.111

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.8277(3) 0.0902(3) 0.5988(2) 0.0242(7) Uani 1 1 d . . . . .
H1A H 0.9057 0.0467 0.6269 0.036 Uiso 1 1 calc R U . . .
H1B H 0.8427 0.1744 0.5816 0.036 Uiso 1 1 calc R U . . .
H1C H 0.7759 0.0479 0.5375 0.036 Uiso 1 1 calc R U . . .
C2 C 0.7646(3) 0.0925(3) 0.6759(2) 0.0169(6) Uani 1 1 d . . . . .
C3 C 0.7948(3) 0.1840(3) 0.7530(2) 0.0159(6) Uani 1 1 d . . . . .
H3 H 0.8616 0.2376 0.7605 0.019 Uiso 1 1 calc R U . . .
C4 C 0.7266(2) 0.1958(3) 0.81816(18) 0.0140(6) Uani 1 1 d . . . . .
H4 H 0.7466 0.2594 0.8675 0.017 Uiso 1 1 calc R U . . .
C5 C 0.6287(3) 0.1152(3) 0.81217(19) 0.0143(6) Uani 1 1 d . . . . .
C6 C 0.6008(3) 0.0240(2) 0.73631(19) 0.0162(6) Uani 1 1 d . . . . .
H6 H 0.536 -0.0316 0.7308 0.019 Uiso 1 1 calc R U . . .
C7 C 0.6663(3) 0.0125(3) 0.66789(19) 0.0161(6) Uani 1 1 d . . . . .
H7 H 0.644 -0.049 0.6168 0.019 Uiso 1 1 calc R U . . .
C8 C 0.5578(3) 0.1250(3) 0.8843(2) 0.0180(6) Uani 1 1 d . . . . .
H8 H 0.4797 0.0785 0.8544 0.022 Uiso 1 1 calc R U . . .
C9 C 0.5266(3) 0.2557(3) 0.9034(2) 0.0268(8) Uani 1 1 d . . . . .
H9A H 0.602 0.3007 0.939 0.04 Uiso 1 1 calc R U . . .
H9B H 0.4741 0.2549 0.945 0.04 Uiso 1 1 calc R U . . .
H9C H 0.4836 0.2959 0.8384 0.04 Uiso 1 1 calc R U . . .
C10 C 0.6336(3) 0.0619(3) 0.9838(2) 0.0220(7) Uani 1 1 d . . . . .
H10A H 0.6472 -0.024 0.9702 0.033 Uiso 1 1 calc R U . . .
H10B H 0.5895 0.0659 1.032 0.033 Uiso 1 1 calc R U . . .
H10C H 0.7125 0.1037 1.0126 0.033 Uiso 1 1 calc R U . . .
C11 C 0.5638(2) 0.3892(2) 0.51397(19) 0.0118(6) Uani 1 1 d . . . . .
C12 C 0.5165(3) 0.4411(2) 0.59344(18) 0.0117(6) Uani 1 1 d . . . . .
C13 C 0.4510(2) 0.5517(2) 0.57810(18) 0.0112(6) Uani 1 1 d . . . . .
C14 C 0.4012(3) 0.6034(3) 0.65397(18) 0.0126(6) Uani 1 1 d . . . . .
C15 C 0.3978(3) 0.7302(3) 0.6685(2) 0.0145(6) Uani 1 1 d . . . . .
H15 H 0.4254 0.7845 0.6279 0.017 Uiso 1 1 calc R U . . .
C16 C 0.3545(3) 0.7771(3) 0.7417(2) 0.0184(6) Uani 1 1 d . . . . .
H16 H 0.3537 0.8633 0.7512 0.022 Uiso 1 1 calc R U . . .
C17 C 0.3127(3) 0.7007(3) 0.8009(2) 0.0206(6) Uani 1 1 d . . . . .
H17 H 0.2827 0.7336 0.8506 0.025 Uiso 1 1 calc R U . . .
C18 C 0.3150(3) 0.5753(3) 0.7869(2) 0.0184(6) Uani 1 1 d . . . . .
H18 H 0.2864 0.5219 0.8275 0.022 Uiso 1 1 calc R U . . .
C19 C 0.3584(3) 0.5264(3) 0.71427(19) 0.0144(6) Uani 1 1 d . . . . .
H19 H 0.359 0.44 0.7055 0.017 Uiso 1 1 calc R U . . .
O1 O 0.62149(17) 0.28841(17) 0.53962(13) 0.0145(4) Uani 1 1 d . . . . .
O2 O 0.54503(18) 0.37858(17) 0.67539(13) 0.0139(4) Uani 1 1 d . . . . .
Cl1 Cl 0.39441(6) 0.16818(7) 0.55912(5) 0.01795(16) Uani 1 1 d . . . . .
Ru1 Ru 0.60277(2) 0.19915(2) 0.66388(2) 0.01048(6) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 1.501(4) . ?
C1 H1A 0.98 . ?
C1 H1B 0.98 . ?
C1 H1C 0.98 . ?
C2 C7 1.413(4) . ?
C2 C3 1.423(4) . ?
C2 Ru1 2.171(3) . ?
C3 C4 1.406(4) . ?
C3 Ru1 2.163(3) . ?
C3 H3 0.95 . ?
C4 C5 1.420(4) . ?
C4 Ru1 2.150(2) . ?
C4 H4 0.95 . ?
C5 C6 1.410(4) . ?
C5 C8 1.511(4) . ?
C5 Ru1 2.195(3) . ?
C6 C7 1.420(4) . ?
C6 Ru1 2.166(3) . ?
C6 H6 0.95 . ?
C7 Ru1 2.159(3) . ?
C7 H7 0.95 . ?
C8 C9 1.516(4) . ?
C8 C10 1.534(4) . ?
C8 H8 1 . ?
C9 H9A 0.98 . ?
C9 H9B 0.98 . ?
C9 H9C 0.98 . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C11 O1 1.274(3) . ?
C11 C13 1.399(3) 3_666 ?
C11 C12 1.511(4) . ?
C12 O2 1.278(3) . ?
C12 C13 1.404(4) . ?
C13 C11 1.399(3) 3_666 ?
C13 C14 1.485(4) . ?
C14 C19 1.398(4) . ?
C14 C15 1.400(4) . ?
C15 C16 1.386(4) . ?
C15 H15 0.95 . ?
C16 C17 1.377(4) . ?
C16 H16 0.95 . ?
C17 C18 1.382(4) . ?
C17 H17 0.95 . ?
C18 C19 1.389(4) . ?
C18 H18 0.95 . ?
C19 H19 0.95 . ?
O1 Ru1 2.0703(18) . ?
O2 Ru1 2.0925(19) . ?
Cl1 Ru1 2.3920(7) . ?

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 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C7 C2 C3 118.5(3) . . ?
C7 C2 C1 121.0(3) . . ?
C3 C2 C1 120.2(3) . . ?
C7 C2 Ru1 70.51(16) . . ?
C3 C2 Ru1 70.52(16) . . ?
C1 C2 Ru1 125.38(19) . . ?
C4 C3 C2 120.6(3) . . ?
C4 C3 Ru1 70.50(15) . . ?
C2 C3 Ru1 71.14(15) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
Ru1 C3 H3 131.5 . . ?
C3 C4 C5 121.7(3) . . ?
C3 C4 Ru1 71.45(14) . . ?
C5 C4 Ru1 72.65(14) . . ?
C3 C4 H4 119.1 . . ?
C5 C4 H4 119.1 . . ?
Ru1 C4 H4 129.2 . . ?
C6 C5 C4 117.0(3) . . ?
C6 C5 C8 121.1(3) . . ?
C4 C5 C8 121.9(2) . . ?
C6 C5 Ru1 70.03(15) . . ?
C4 C5 Ru1 69.23(14) . . ?
C8 C5 Ru1 132.36(19) . . ?
C5 C6 C7 122.2(3) . . ?
C5 C6 Ru1 72.25(16) . . ?
C7 C6 Ru1 70.57(15) . . ?
C5 C6 H6 118.9 . . ?
C7 C6 H6 118.9 . . ?
Ru1 C6 H6 131.3 . . ?
C2 C7 C6 119.9(2) . . ?
C2 C7 Ru1 71.39(16) . . ?
C6 C7 Ru1 71.10(15) . . ?
C2 C7 H7 120 . . ?
C6 C7 H7 120 . . ?
Ru1 C7 H7 130 . . ?
C5 C8 C9 113.8(2) . . ?
C5 C8 C10 107.5(2) . . ?
C9 C8 C10 111.0(2) . . ?
C5 C8 H8 108.1 . . ?
C9 C8 H8 108.1 . . ?
C10 C8 H8 108.1 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O1 C11 C13 123.0(2) . 3_666 ?
O1 C11 C12 113.9(2) . . ?
C13 C11 C12 123.1(2) 3_666 . ?
O2 C12 C13 123.8(2) . . ?
O2 C12 C11 114.5(2) . . ?
C13 C12 C11 121.6(2) . . ?
C11 C13 C12 115.2(2) 3_666 . ?
C11 C13 C14 122.0(2) 3_666 . ?
C12 C13 C14 122.7(2) . . ?
C19 C14 C15 118.1(2) . . ?
C19 C14 C13 120.8(2) . . ?
C15 C14 C13 121.1(2) . . ?
C16 C15 C14 120.5(3) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C17 C16 C15 121.0(3) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C16 C17 C18 119.0(3) . . ?
C16 C17 H17 120.5 . . ?
C18 C17 H17 120.5 . . ?
C17 C18 C19 120.9(3) . . ?
C17 C18 H18 119.6 . . ?
C19 C18 H18 119.6 . . ?
C18 C19 C14 120.4(3) . . ?
C18 C19 H19 119.8 . . ?
C14 C19 H19 119.8 . . ?
C11 O1 Ru1 116.48(17) . . ?
C12 O2 Ru1 114.90(16) . . ?
O1 Ru1 O2 75.79(7) . . ?
O1 Ru1 C4 128.78(9) . . ?
O2 Ru1 C4 93.50(9) . . ?
O1 Ru1 C7 109.35(9) . . ?
O2 Ru1 C7 174.37(8) . . ?
C4 Ru1 C7 81.48(10) . . ?
O1 Ru1 C3 97.82(9) . . ?
O2 Ru1 C3 108.83(9) . . ?
C4 Ru1 C3 38.05(10) . . ?
C7 Ru1 C3 68.64(11) . . ?
O1 Ru1 C6 146.04(9) . . ?
O2 Ru1 C6 137.11(9) . . ?
C4 Ru1 C6 67.97(10) . . ?
C7 Ru1 C6 38.33(11) . . ?
C3 Ru1 C6 80.61(11) . . ?
O1 Ru1 C2 88.79(9) . . ?
O2 Ru1 C2 141.97(10) . . ?
C4 Ru1 C2 69.31(10) . . ?
C7 Ru1 C2 38.10(11) . . ?
C3 Ru1 C2 38.34(10) . . ?
C6 Ru1 C2 68.88(11) . . ?
O1 Ru1 C5 166.49(9) . . ?
O2 Ru1 C5 105.11(9) . . ?
C4 Ru1 C5 38.12(10) . . ?
C7 Ru1 C5 69.35(10) . . ?
C3 Ru1 C5 68.98(11) . . ?
C6 Ru1 C5 37.72(10) . . ?
C2 Ru1 C5 82.44(10) . . ?
O1 Ru1 Cl1 85.78(6) . . ?
O2 Ru1 Cl1 83.91(6) . . ?
C4 Ru1 Cl1 143.68(8) . . ?
C7 Ru1 Cl1 98.60(8) . . ?
C3 Ru1 Cl1 167.23(8) . . ?
C6 Ru1 Cl1 89.55(8) . . ?
C2 Ru1 Cl1 130.07(8) . . ?
C5 Ru1 Cl1 107.72(8) . . ?


#----------------------------------------------------------------------------#
#                   SQUEEZE DETAILS                                          #
#----------------------------------------------------------------------------#


# END of CIF

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloromethane/MeOH'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_TC_252_TCE_hept_synchrotron_data
_database_code_depnum_ccdc_archive 'CCDC 2264977'
loop_
_audit_author_name
_audit_author_address
'Werner Kaminsky'
;University of Washington
United States of America
;
_audit_update_record             
;
2023-07-07 deposited with the CCDC.	2023-08-17 downloaded from the CCDC.
;

_audit_creation_date             2023-07-06T15:54:15-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.5
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C72 H44 F4 [+solvent]'
_chemical_formula_sum            'C72 H44 F4'
_chemical_formula_weight         985.07

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   19.7037(19)
_cell_length_b                   8.3789(8)
_cell_length_c                   21.004(2)
_cell_angle_alpha                90
_cell_angle_beta                 108.289(3)
_cell_angle_gamma                90
_cell_volume                     3292.4(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4164
_cell_measurement_theta_min      2.66
_cell_measurement_theta_max      26.33
_cell_measurement_wavelength     0.7288

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_exptl_crystal_density_diffrn    0.994
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1024

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        TWINABS - Bruker AXS scaling for twinned crystals - Version 2012/1
;
_exptl_absorpt_correction_T_min  0.587
_exptl_absorpt_correction_T_max  0.745
_shelx_estimated_absorpt_T_min   0.98
_shelx_estimated_absorpt_T_max   0.997

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'ALS-U Lawrence Berkeley National Laboratory'
_diffrn_source_type              'ALS-U Beamline 12.2.1'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7288
_diffrn_radiation_type           synchrotron
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'APEX-II CCD'
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'φ or ω oscillation scans'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_number            6324
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.041
_diffrn_reflns_theta_max         27.106
_diffrn_reflns_theta_full        25.93
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.935
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.935
_reflns_Friedel_coverage         0
_reflns_number_total             6324
_reflns_number_gt                5358
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2 software'
_computing_cell_refinement       'SAINT V8.40B integration software'
_computing_data_reduction        'SORTAV (Blessing, 1995)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_shelx_SHELXL_version_number     2019/3
_refine_special_details          
;
 Refined as a 2-component twin.
The twin law is a two-fold rotation 
about [0 0 1] with twin fraction of
0.258(2), refined from hklf 5 data.

;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1591P)²+1.1411P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6324
_refine_ls_number_parameters     362
_refine_ls_number_restraints     180
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0706
_refine_ls_wR_factor_ref         0.224
_refine_ls_wR_factor_gt          0.2148
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.02
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.063

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0024 0.0017 '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'
F F 0.0146 0.0109 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.04585(15) 0.7554(4) 0.22064(16) 0.0427(7) Uani 1 1 d D . . . .
C2 C 0.07436(17) 0.7611(4) 0.16739(17) 0.0503(8) Uani 1 1 d D . . . .
H2 H 0.044056 0.787228 0.1237 0.06 Uiso 0.5 1 calc R U P A 2
C3 C 0.14563(17) 0.7296(4) 0.17727(17) 0.0513(8) Uani 1 1 d D . . . .
H3 H 0.163081 0.735869 0.140007 0.062 Uiso 0.5 1 calc R U P B 2
C4 C 0.19275(15) 0.6891(3) 0.23935(15) 0.0407(6) Uani 1 1 d D . . . .
C5 C 0.16527(15) 0.6970(4) 0.29376(15) 0.0423(6) Uani 1 1 d D . . . .
H5 H 0.196397 0.680817 0.33807 0.051 Uiso 0.5 1 calc R U P C 2
C6 C 0.09412(15) 0.7277(4) 0.28355(17) 0.0471(7) Uani 1 1 d D . . . .
H6 H 0.077346 0.729956 0.321294 0.057 Uiso 0.5 1 calc R U P D 2
C7 C 0.26426(14) 0.6204(3) 0.24545(15) 0.0396(6) Uani 1 1 d D . . . .
C8 C 0.30138(15) 0.6617(4) 0.20100(17) 0.0436(7) Uani 1 1 d D . . . .
H8 H 0.289005 0.756786 0.175341 0.052 Uiso 1 1 calc R U . . .
C9 C 0.35610(15) 0.5659(3) 0.19373(16) 0.0410(6) Uani 1 1 d D . . . .
H9 H 0.379562 0.595015 0.162242 0.049 Uiso 1 1 calc R U . . .
C10 C 0.37721(14) 0.4272(3) 0.23200(14) 0.0358(6) Uani 1 1 d D . . . .
C11 C 0.34621(14) 0.3982(3) 0.28271(14) 0.0375(6) Uani 1 1 d D . . . .
H11 H 0.363438 0.312532 0.313138 0.045 Uiso 1 1 calc R U . . .
C12 C 0.29095(14) 0.4925(4) 0.28905(15) 0.0398(6) Uani 1 1 d D . . . .
H12 H 0.270764 0.469949 0.323626 0.048 Uiso 1 1 calc R U . . .
C13 C 0.41843(14) 0.3022(3) 0.20935(14) 0.0347(6) Uani 1 1 d D . . . .
C14 C 0.45725(14) 0.3374(3) 0.16620(15) 0.0370(6) Uani 1 1 d D . . . .
H14 H 0.47158 0.444432 0.162674 0.044 Uiso 1 1 calc R U . . .
C15 C 0.47551(14) 0.2198(3) 0.12822(14) 0.0352(6) Uani 1 1 d D . . . .
H15 H 0.500197 0.24792 0.097587 0.042 Uiso 1 1 calc R U . . .
C16 C 0.45795(13) 0.0597(3) 0.13446(14) 0.0351(6) Uani 1 1 d D . . . .
C17 C 0.42899(14) 0.0215(3) 0.18529(14) 0.0366(6) Uani 1 1 d D . . . .
H17 H 0.423076 -0.087356 0.195071 0.044 Uiso 1 1 calc R U . . .
C18 C 0.40884(14) 0.1396(3) 0.22155(14) 0.0359(6) Uani 1 1 d D . . . .
H18 H 0.388207 0.110862 0.255183 0.043 Uiso 1 1 calc R U . . .
C19 C 0.45635(14) -0.0627(3) 0.08283(13) 0.0335(6) Uani 1 1 d D . . . .
C20 C 0.42036(15) -0.0280(3) 0.01510(14) 0.0377(6) Uani 1 1 d D . . . .
H20 H 0.410692 0.080058 0.001557 0.045 Uiso 1 1 calc R U . . .
C21 C 0.39878(14) -0.1480(3) -0.03219(14) 0.0384(6) Uani 1 1 d D . . . .
H21 H 0.37345 -0.121296 -0.07738 0.046 Uiso 1 1 calc R U . . .
C22 C 0.41373(13) -0.3080(3) -0.01438(13) 0.0337(6) Uani 1 1 d D . . . .
C23 C 0.45933(14) -0.3399(3) 0.05022(14) 0.0355(6) Uani 1 1 d D . . . .
H23 H 0.477094 -0.445007 0.061536 0.043 Uiso 1 1 calc R U . . .
C24 C 0.47893(13) -0.2199(3) 0.09796(14) 0.0353(6) Uani 1 1 d D . . . .
H24 H 0.508448 -0.245366 0.14202 0.042 Uiso 1 1 calc R U . . .
C25 C 0.37137(14) -0.4356(3) -0.05823(14) 0.0359(6) Uani 1 1 d D . . . .
C26 C 0.34336(14) -0.4246(3) -0.12762(14) 0.0380(6) Uani 1 1 d D . . . .
H26 H 0.36334 -0.350417 -0.150962 0.046 Uiso 1 1 calc R U . . .
C27 C 0.28645(14) -0.5206(4) -0.16351(15) 0.0402(6) Uani 1 1 d D . . . .
H27 H 0.268417 -0.510631 -0.210918 0.048 Uiso 1 1 calc R U . . .
C28 C 0.25536(14) -0.6311(3) -0.13135(15) 0.0401(6) Uani 1 1 d D . . . .
C29 C 0.29091(17) -0.6571(4) -0.06351(17) 0.0489(8) Uani 1 1 d D . . . .
H29 H 0.27548 -0.741553 -0.041175 0.059 Uiso 1 1 calc R U . . .
C30 C 0.34767(16) -0.5642(4) -0.02796(16) 0.0469(7) Uani 1 1 d D . . . .
H30 H 0.371276 -0.587405 0.017945 0.056 Uiso 1 1 calc R U . . .
C31 C 0.18230(15) -0.6978(3) -0.16377(16) 0.0430(7) Uani 1 1 d D . . . .
C32 C 0.13678(15) -0.6288(4) -0.22281(16) 0.0478(7) Uani 1 1 d D . . . .
H32 H 0.156025 -0.560215 -0.248806 0.057 Uiso 1 1 calc R U . . .
C33 C 0.06375(15) -0.6604(4) -0.24344(17) 0.0479(7) Uani 1 1 d D . . . .
H33 H 0.034247 -0.612911 -0.283693 0.058 Uiso 1 1 calc R U . . .
C34 C 0.03267(14) -0.7580(4) -0.20759(17) 0.0440(7) Uani 1 1 d D . . . .
C35 C 0.07946(17) -0.8410(4) -0.1528(2) 0.0561(9) Uani 1 1 d D . . . .
H35 H 0.060891 -0.917584 -0.129257 0.067 Uiso 1 1 calc R U . . .
C36 C 0.15224(17) -0.8116(4) -0.13310(19) 0.0544(8) Uani 1 1 d D . . . .
H36 H 0.182752 -0.871836 -0.097114 0.065 Uiso 1 1 calc R U . . .
F1 F 0.0742(2) 0.7413(7) 0.3399(2) 0.0722(12) Uani 0.5 1 d . . P E 1
F2 F 0.2086(2) 0.6802(5) 0.3579(2) 0.0632(10) Uani 0.5 1 d . . P F 1
F3 F 0.1632(3) 0.7117(9) 0.1234(2) 0.0893(18) Uani 0.5 1 d . . P G 1
F4 F 0.0288(3) 0.7760(8) 0.1050(3) 0.0858(16) Uani 0.5 1 d . . P H 1



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 C6 1.384(5) . ?
C1 C2 1.401(4) . ?
C1 C34 1.484(4) 3 ?
C2 F4 1.341(6) . ?
C2 C3 1.379(4) . ?
C2 H2 0.95 . ?
C3 F3 1.292(6) . ?
C3 C4 1.385(5) . ?
C3 H3 0.95 . ?
C4 C5 1.411(4) . ?
C4 C7 1.490(4) . ?
C5 F2 1.358(5) . ?
C5 C6 1.374(4) . ?
C5 H5 0.95 . ?
C6 F1 1.363(6) . ?
C6 H6 0.95 . ?
C7 C8 1.398(4) . ?
C7 C12 1.400(4) . ?
C8 C9 1.391(4) . ?
C8 H8 0.95 . ?
C9 C10 1.400(4) . ?
C9 H9 0.95 . ?
C10 C11 1.405(4) . ?
C10 C13 1.492(4) . ?
C11 C12 1.385(4) . ?
C11 H11 0.95 . ?
C12 H12 0.95 . ?
C13 C14 1.389(4) . ?
C13 C18 1.410(4) . ?
C14 C15 1.385(4) . ?
C14 H14 0.95 . ?
C15 C16 1.402(4) . ?
C15 H15 0.95 . ?
C16 C17 1.396(4) . ?
C16 C19 1.486(4) . ?
C17 C18 1.381(4) . ?
C17 H17 0.95 . ?
C18 H18 0.95 . ?
C19 C24 1.395(4) . ?
C19 C20 1.407(4) . ?
C20 C21 1.383(4) . ?
C20 H20 0.95 . ?
C21 C22 1.398(4) . ?
C21 H21 0.95 . ?
C22 C23 1.398(4) . ?
C22 C25 1.485(4) . ?
C23 C24 1.386(4) . ?
C23 H23 0.95 . ?
C24 H24 0.95 . ?
C25 C26 1.390(4) . ?
C25 C30 1.403(4) . ?
C26 C27 1.394(4) . ?
C26 H26 0.95 . ?
C27 C28 1.396(4) . ?
C27 H27 0.95 . ?
C28 C29 1.394(4) . ?
C28 C31 1.494(4) . ?
C29 C30 1.375(4) . ?
C29 H29 0.95 . ?
C30 H30 0.95 . ?
C31 C36 1.384(5) . ?
C31 C32 1.406(4) . ?
C32 C33 1.392(4) . ?
C32 H32 0.95 . ?
C33 C34 1.378(5) . ?
C33 H33 0.95 . ?
C34 C35 1.412(5) . ?
C35 C36 1.384(4) . ?
C35 H35 0.95 . ?
C36 H36 0.95 . ?

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
C6 C1 C2 116.1(3) . . ?
C6 C1 C34 122.9(3) . 3 ?
C2 C1 C34 120.5(3) . 3 ?
F4 C2 C3 120.2(4) . . ?
F4 C2 C1 118.0(3) . . ?
C3 C2 C1 121.2(3) . . ?
C3 C2 H2 119.4 . . ?
C1 C2 H2 119.4 . . ?
F3 C3 C2 115.5(4) . . ?
F3 C3 C4 120.8(3) . . ?
C2 C3 C4 122.6(3) . . ?
C2 C3 H3 118.7 . . ?
C4 C3 H3 118.7 . . ?
C3 C4 C5 115.9(3) . . ?
C3 C4 C7 120.8(3) . . ?
C5 C4 C7 122.8(3) . . ?
F2 C5 C6 117.8(3) . . ?
F2 C5 C4 121.2(3) . . ?
C6 C5 C4 121.0(3) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
F1 C6 C5 115.9(3) . . ?
F1 C6 C1 121.1(3) . . ?
C5 C6 C1 122.8(3) . . ?
C5 C6 H6 118.6 . . ?
C1 C6 H6 118.6 . . ?
C8 C7 C12 117.3(2) . . ?
C8 C7 C4 121.7(3) . . ?
C12 C7 C4 120.2(2) . . ?
C9 C8 C7 121.1(3) . . ?
C9 C8 H8 119.5 . . ?
C7 C8 H8 119.5 . . ?
C8 C9 C10 121.1(3) . . ?
C8 C9 H9 119.4 . . ?
C10 C9 H9 119.4 . . ?
C9 C10 C11 117.2(2) . . ?
C9 C10 C13 119.5(3) . . ?
C11 C10 C13 122.0(2) . . ?
C12 C11 C10 121.1(3) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.5 . . ?
C11 C12 C7 121.3(3) . . ?
C11 C12 H12 119.4 . . ?
C7 C12 H12 119.4 . . ?
C14 C13 C18 117.2(2) . . ?
C14 C13 C10 121.7(2) . . ?
C18 C13 C10 120.2(2) . . ?
C15 C14 C13 121.4(2) . . ?
C15 C14 H14 119.3 . . ?
C13 C14 H14 119.3 . . ?
C14 C15 C16 120.7(2) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 H15 119.6 . . ?
C17 C16 C15 117.6(2) . . ?
C17 C16 C19 118.7(2) . . ?
C15 C16 C19 122.8(2) . . ?
C18 C17 C16 121.0(3) . . ?
C18 C17 H17 119.5 . . ?
C16 C17 H17 119.5 . . ?
C17 C18 C13 120.9(2) . . ?
C17 C18 H18 119.5 . . ?
C13 C18 H18 119.5 . . ?
C24 C19 C20 116.7(2) . . ?
C24 C19 C16 123.6(2) . . ?
C20 C19 C16 118.9(2) . . ?
C21 C20 C19 121.3(3) . . ?
C21 C20 H20 119.3 . . ?
C19 C20 H20 119.3 . . ?
C20 C21 C22 120.9(3) . . ?
C20 C21 H21 119.6 . . ?
C22 C21 H21 119.6 . . ?
C23 C22 C21 117.4(2) . . ?
C23 C22 C25 121.9(2) . . ?
C21 C22 C25 119.6(2) . . ?
C24 C23 C22 120.8(2) . . ?
C24 C23 H23 119.6 . . ?
C22 C23 H23 119.6 . . ?
C23 C24 C19 121.6(2) . . ?
C23 C24 H24 119.2 . . ?
C19 C24 H24 119.2 . . ?
C26 C25 C30 116.5(3) . . ?
C26 C25 C22 124.3(3) . . ?
C30 C25 C22 118.3(3) . . ?
C25 C26 C27 121.1(3) . . ?
C25 C26 H26 119.5 . . ?
C27 C26 H26 119.5 . . ?
C26 C27 C28 121.5(3) . . ?
C26 C27 H27 119.3 . . ?
C28 C27 H27 119.3 . . ?
C29 C28 C27 116.3(3) . . ?
C29 C28 C31 120.7(3) . . ?
C27 C28 C31 122.3(3) . . ?
C30 C29 C28 121.9(3) . . ?
C30 C29 H29 119 . . ?
C28 C29 H29 119 . . ?
C29 C30 C25 121.2(3) . . ?
C29 C30 H30 119.4 . . ?
C25 C30 H30 119.4 . . ?
C36 C31 C32 116.5(3) . . ?
C36 C31 C28 122.5(3) . . ?
C32 C31 C28 120.3(3) . . ?
C33 C32 C31 120.5(3) . . ?
C33 C32 H32 119.7 . . ?
C31 C32 H32 119.7 . . ?
C34 C33 C32 122.4(3) . . ?
C34 C33 H33 118.8 . . ?
C32 C33 H33 118.8 . . ?
C33 C34 C35 116.7(3) . . ?
C33 C34 C1 120.4(3) . 3 ?
C35 C34 C1 122.3(3) . 3 ?
C36 C35 C34 120.4(3) . . ?
C36 C35 H35 119.8 . . ?
C34 C35 H35 119.8 . . ?
C31 C36 C35 122.6(3) . . ?
C31 C36 H36 118.7 . . ?
C35 C36 H36 118.7 . . ?


#----------------------------------------------------------------------------#
#                   SQUEEZE DETAILS                                          #
#----------------------------------------------------------------------------#


# END of CIF

_chemical_name_systematic        tetrafluoro[12]cycloparaphenylene
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: trichloroethylene/n-heptane'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_AAK_4245_4_TCE_hept
_database_code_depnum_ccdc_archive 'CCDC 2264976'
loop_
_audit_author_name
_audit_author_address
'Werner Kaminsky'
;University of Washington
United States of America
;
_audit_update_record             
;
2023-05-23 deposited with the CCDC.	2023-08-17 downloaded from the CCDC.
;

_audit_creation_date             2023-04-17T15:09:29-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.5
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C76 H56 O4, C2 H Cl3 [+ solvent]'
_chemical_formula_sum            'C78 H57 Cl3 O4'
_chemical_formula_weight         1164.58
_chemical_absolute_configuration unk

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_Int_Tables_number      43
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'

_cell_length_a                   57.683(4)
_cell_length_b                   12.1111(8)
_cell_length_c                   50.915(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     35569(4)
_cell_formula_units_Z            16
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9981
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      24.76
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_exptl_crystal_density_diffrn    0.87
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             9728

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.139
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        SADABS-2016/2 - Bruker AXS area detector scaling and absorption correcti
;
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_T_max  0.958
_shelx_estimated_absorpt_T_min   0.921
_shelx_estimated_absorpt_T_max   0.988

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'sealed x-ray tube'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'APEX-II CCD'
_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_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       'φ or ω oscillation scans'
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.1097
_diffrn_reflns_av_unetI/netI     0.09
_diffrn_reflns_number            101139
_diffrn_reflns_limit_h_min       -68
_diffrn_reflns_limit_h_max       68
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_theta_min         2.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_full        25.027
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.994
_reflns_Friedel_coverage         0.978
_reflns_number_total             15535
_reflns_number_gt                9099
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2 software'
_computing_cell_refinement       'SAINT V8.38A integration software'
_computing_data_reduction        'SORTAV (Blessing, 1995)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_shelx_SHELXL_version_number     2014/7
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1793P)²+212.6177P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         15535
_refine_ls_number_parameters     786
_refine_ls_number_restraints     1003
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.18
_refine_ls_R_factor_gt           0.1202
_refine_ls_wR_factor_ref         0.3545
_refine_ls_wR_factor_gt          0.3064
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.6(2)
_refine_diff_density_max         0.43
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.077

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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_
_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



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 . ?

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 . . ?



# END of CIF

_chemical_name_common            tetramethoxy[12]cycloparaphenylene
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: trichloroethylene/n-heptane'
