#------------------------------------------------------------------------------
#$Date: 2021-02-04 02:58:15 +0200 (Thu, 04 Feb 2021) $
#$Revision: 261481 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/56/4135616.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4135616
loop_
_publ_author_name
'Mi, Yan'
'Ma, Jingyu'
'Liang, Wenting'
'Xiao, Chao'
'Wu, Wanhua'
'Zhou, Dayang'
'Yao, Jiabin'
'Sun, Wenjia'
'Sun, Junliang'
'Gao, Guowei'
'Chen, Xiaochuan'
'Chruma, Jason J.'
'Yang, Cheng'
_publ_section_title
;
 Guest-Binding-Induced Interhetero Hosts Charge Transfer Crystallization:
 Selective Coloration of Commonly Used Organic Solvents.
;
_journal_issue                   3
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1553
_journal_page_last               1561
_journal_paper_doi               10.1021/jacs.0c11833
_journal_volume                  143
_journal_year                    2021
_chemical_formula_moiety
'2(C45 H50 O10), 2(C35 H20 O10), 4(C2 H4 O2), 2(C4 H7 O2)'
_chemical_formula_sum            'C176 H172 O48'
_chemical_formula_weight         3055.13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-11-29
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_cell_angle_alpha                68.21
_cell_angle_beta                 89.91
_cell_angle_gamma                73.20
_cell_formula_units_Z            1
_cell_length_a                   12.182
_cell_length_b                   17.093
_cell_length_c                   21.861
_cell_measurement_reflns_used    15326
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.4850
_cell_measurement_theta_min      2.1800
_cell_volume                     4017.687
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  ' '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            58741
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.726
_diffrn_reflns_theta_min         1.010
_exptl_absorpt_coefficient_mu    0.092
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       ' '
_exptl_crystal_F_000             1612
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1043
_refine_ls_number_reflns         16259
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      49.204
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0731
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1278P)²+1.3052P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2179
_refine_ls_wR_factor_ref         0.2400
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11227
_reflns_number_total             16259
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja0c11833_si_002.cif
_cod_data_source_block           08
_cod_original_cell_volume        4017.6
_cod_database_code               4135616
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C88-C89
 1.42 with sigma of 0.005
 O26-O23
 2.04 with sigma of 0.001
 C7-O13 \\sim C71-O5 \\sim C88-O26
 with sigma of 0.001
 C85-O26 \\sim C89-O26
 with sigma of 0.001
3.a Secondary CH2 refined with riding coordinates:
 C10(H10a,H10b), C31(H31a,H31b), C35(H35a,H35b), C36(H36a,H36b), C37(H37a,
 H37b), C44(H44a,H44b), C45(H45a,H45b), C49(H49a,H49b), C70(H70a,H70b),
 C72(H72a,H72b)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C16(H16), C17(H17), C20(H20), C26(H26), C27(H27), C32(H32), C39(H39),
 C40(H40), C41(H41), C42(H42), C43(H43), C51(H51), C52(H52), C54(H54), C58(H58),
  C60(H60), C64(H64), C67(H67), C68(H68), C88(H88)
3.c Idealised Me refined as rotating group:
 C69(H69a,H69b,H69c), C71(H71a,H71b,H71c), C73(H73a,H73b,H73c), C74(H74a,H74b,
 H74c), C75(H75a,H75b,H75c), C76(H76a,H76b,H76c), C77(H77a,H77b,H77c), C79(H79a,
 H79b,H79c), C80(H80a,H80b,H80c), C83(H83a,H83b,H83c), C84(H84a,H84b,H84c),
 C85(H85a,H85b,H85c), C87(H87a,H87b,H87c), C89(H89a,H89b,H89c)
3.d Idealised tetrahedral OH refined as rotating group:
 O22(H22), O24(H24)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.77253(16) 0.47379(12) 0.20000(9) 0.0612(5) Uani 1 1 d . . . . .
O2 O -0.01943(18) 0.56627(12) 0.22796(9) 0.0668(5) Uani 1 1 d . . . . .
O3 O 0.26490(16) 0.25413(13) 0.26512(10) 0.0655(5) Uani 1 1 d . . . . .
O4 O 0.64274(17) 0.24617(12) 0.37184(10) 0.0638(5) Uani 1 1 d . . . . .
O5 O 0.17136(19) 0.47173(14) 0.02660(10) 0.0700(5) Uani 1 1 d D . . . .
O6 O 0.25481(17) 0.42086(14) 0.43941(10) 0.0683(5) Uani 1 1 d . . . . .
O7 O 0.78745(17) 0.33809(13) 0.51626(11) 0.0685(5) Uani 1 1 d . . . . .
O8 O 0.98367(19) -0.18935(13) 0.71350(11) 0.0754(6) Uani 1 1 d . . . . .
O9 O 1.17706(18) 0.17257(14) 0.45341(10) 0.0701(5) Uani 1 1 d . . . . .
O10 O 0.65347(19) 0.10418(15) 0.68420(11) 0.0775(6) Uani 1 1 d . . . . .
O11 O 0.55760(19) 0.57814(14) 0.37816(13) 0.0798(6) Uani 1 1 d . . . . .
O12 O 1.14411(19) 0.34881(16) 0.61024(12) 0.0805(6) Uani 1 1 d . . . . .
O13 O 0.50741(18) 0.62579(17) -0.02113(11) 0.0807(6) Uani 1 1 d D . . . .
O14 O 1.4542(2) 0.03696(15) 0.65725(12) 0.0843(7) Uani 1 1 d . . . . .
O15 O 0.8513(2) 0.03853(15) 0.48276(12) 0.0821(6) Uani 1 1 d . . . . .
O16 O 0.08625(18) 0.79066(14) 0.04053(14) 0.0840(7) Uani 1 1 d . . . . .
O17 O 0.4610(2) 0.80735(14) 0.13913(11) 0.0889(7) Uani 1 1 d . . . . .
C1 C 0.1641(2) 0.36061(15) 0.30586(11) 0.0463(5) Uani 1 1 d . . . . .
O18 O 1.2351(3) 0.11660(17) 0.84519(12) 0.1023(9) Uani 1 1 d . . . . .
O19 O 1.3340(2) -0.19187(17) 0.82249(14) 0.0945(7) Uani 1 1 d . . . . .
C2 C 0.3570(2) 0.31666(15) 0.39730(12) 0.0475(5) Uani 1 1 d . . . . .
C3 C 0.1160(2) 0.43089(16) 0.13854(12) 0.0496(5) Uani 1 1 d . . . . .
H3 H 0.143638 0.371037 0.145882 0.060 Uiso 1 1 calc R . . . .
C4 C 0.7482(2) 0.00608(17) 0.63438(12) 0.0499(5) Uani 1 1 d . . . . .
C5 C 0.6649(2) 0.46849(16) 0.34249(11) 0.0472(5) Uani 1 1 d . . . . .
C6 C 1.2630(2) 0.23991(16) 0.57599(12) 0.0479(5) Uani 1 1 d . . . . .
C7 C 0.6728(2) 0.58797(16) 0.23344(11) 0.0471(5) Uani 1 1 d D . . . .
C8 C 0.5637(2) 0.69503(17) 0.10422(12) 0.0517(6) Uani 1 1 d . . . . .
C9 C 0.06838(19) 0.45537(15) 0.18882(11) 0.0455(5) Uani 1 1 d . . . . .
C10 C 0.0617(2) 0.38670(15) 0.25515(11) 0.0470(5) Uani 1 1 d . . . . .
H10A H 0.057376 0.334264 0.248987 0.056 Uiso 1 1 calc R . . . .
H10B H -0.008621 0.409810 0.272199 0.056 Uiso 1 1 calc R . . . .
C11 C 1.0614(2) 0.28618(17) 0.48361(12) 0.0503(5) Uani 1 1 d . . . . .
C12 C 0.2657(2) 0.29447(16) 0.30921(12) 0.0486(5) Uani 1 1 d . . . . .
C13 C 0.6959(2) 0.55761(16) 0.18289(12) 0.0487(5) Uani 1 1 d . . . . .
C14 C 0.2542(2) 0.38161(16) 0.39470(12) 0.0491(5) Uani 1 1 d . . . . .
C15 C 0.1238(2) 0.49350(17) 0.07723(12) 0.0504(6) Uani 1 1 d . . . . .
C16 C 0.1602(2) 0.40246(15) 0.34953(12) 0.0497(5) Uani 1 1 d . . . . .
H16 H 0.092501 0.445834 0.348571 0.060 Uiso 1 1 calc R . . . .
C17 C 0.3594(2) 0.27353(16) 0.35424(12) 0.0516(6) Uani 1 1 d . . . . .
H17 H 0.426269 0.229097 0.355837 0.062 Uiso 1 1 calc R . . . .
C18 C 1.1698(2) 0.21595(17) 0.48739(12) 0.0512(6) Uani 1 1 d . . . . .
C19 C 0.8899(2) 0.24285(17) 0.46583(11) 0.0486(5) Uani 1 1 d . . . . .
C20 C 0.6417(2) 0.61059(17) 0.11895(12) 0.0512(6) Uani 1 1 d . . . . .
H20 H 0.657558 0.589488 0.085295 0.061 Uiso 1 1 calc R . . . .
C21 C 0.6235(2) 0.32971(16) 0.37242(12) 0.0484(5) Uani 1 1 d . . . . .
C22 C 0.1986(2) 0.68296(17) 0.00414(11) 0.0542(6) Uani 1 1 d . . . . .
C23 C 0.74820(19) 0.13361(17) 0.53269(11) 0.0479(5) Uani 1 1 d . . . . .
C24 C 0.0823(2) 0.58350(17) 0.06493(12) 0.0507(6) Uani 1 1 d . . . . .
C25 C 0.5366(2) 0.35515(16) 0.40950(12) 0.0490(5) Uani 1 1 d . . . . .
C26 C 0.6867(2) 0.38529(17) 0.34057(11) 0.0500(5) Uani 1 1 d . . . . .
H26 H 0.745422 0.366347 0.317218 0.060 Uiso 1 1 calc R . . . .
C27 C 1.2681(2) 0.19819(17) 0.53508(12) 0.0509(6) Uani 1 1 d . . . . .
H27 H 1.337049 0.155660 0.536557 0.061 Uiso 1 1 calc R . . . .
C28 C 0.8019(2) 0.26987(17) 0.50738(12) 0.0519(6) Uani 1 1 d . . . . .
C29 C 0.0264(2) 0.54562(16) 0.17632(12) 0.0503(6) Uani 1 1 d . . . . .
C30 C 0.3977(2) 0.72893(17) 0.02059(11) 0.0542(6) Uani 1 1 d . . . . .
C31 C 0.7311(2) 0.53047(17) 0.30440(11) 0.0493(5) Uani 1 1 d . . . . .
H31A H 0.809085 0.495849 0.303041 0.059 Uiso 1 1 calc R . . . .
H31B H 0.736145 0.568442 0.327343 0.059 Uiso 1 1 calc R . . . .
O20 O 0.9337(3) -0.0443(2) 0.88946(15) 0.1086(9) Uani 1 1 d . . . . .
C32 C 0.7339(2) 0.20989(17) 0.53914(12) 0.0529(6) Uani 1 1 d . . . . .
H32 H 0.678256 0.226493 0.564953 0.064 Uiso 1 1 calc R . . . .
C33 C 0.5784(2) 0.49428(17) 0.37891(13) 0.0545(6) Uani 1 1 d . . . . .
C34 C 1.3544(2) 0.15024(17) 0.69215(12) 0.0512(6) Uani 1 1 d . . . . .
C35 C 1.3607(2) 0.22057(18) 0.62712(13) 0.0551(6) Uani 1 1 d . . . . .
H35A H 1.433831 0.201069 0.611169 0.066 Uiso 1 1 calc R . . . .
H35B H 1.356986 0.274389 0.633595 0.066 Uiso 1 1 calc R . . . .
C36 C 0.4631(2) 0.29736(17) 0.44254(12) 0.0531(6) Uani 1 1 d . . . . .
H36A H 0.508615 0.235592 0.455747 0.064 Uiso 1 1 calc R . . . .
H36B H 0.439810 0.306981 0.482279 0.064 Uiso 1 1 calc R . . . .
C37 C 0.9608(2) 0.3034(2) 0.43503(12) 0.0594(7) Uani 1 1 d . . . . .
H37A H 0.912517 0.364549 0.421072 0.071 Uiso 1 1 calc R . . . .
H37B H 0.989434 0.294042 0.396048 0.071 Uiso 1 1 calc R . . . .
C38 C 1.1539(2) 0.30894(18) 0.57314(13) 0.0550(6) Uani 1 1 d . . . . .
C39 C 0.8301(2) -0.06960(18) 0.64419(13) 0.0577(6) Uani 1 1 d . . . . .
H39 H 0.844602 -0.086993 0.608620 0.069 Uiso 1 1 calc R . . . .
C40 C 0.0324(2) 0.60782(16) 0.11503(12) 0.0546(6) Uani 1 1 d . . . . .
H40 H 0.002051 0.667715 0.107157 0.065 Uiso 1 1 calc R . . . .
C41 C 0.5951(2) 0.67115(17) 0.21943(12) 0.0556(6) Uani 1 1 d . . . . .
H41 H 0.579368 0.692018 0.253210 0.067 Uiso 1 1 calc R . . . .
C42 C 1.0568(2) 0.32820(19) 0.52445(13) 0.0577(6) Uani 1 1 d . . . . .
H42 H 0.988569 0.371985 0.522087 0.069 Uiso 1 1 calc R . . . .
C43 C 0.9033(2) 0.16686(18) 0.45880(12) 0.0551(6) Uani 1 1 d . . . . .
H43 H 0.958210 0.150531 0.432507 0.066 Uiso 1 1 calc R . . . .
C44 C 0.5042(2) 0.75100(18) 0.03383(12) 0.0577(6) Uani 1 1 d . . . . .
H44A H 0.482852 0.813202 0.026825 0.069 Uiso 1 1 calc R . . . .
H44B H 0.557844 0.741257 0.002585 0.069 Uiso 1 1 calc R . . . .
C45 C 0.6838(2) 0.06927(19) 0.56706(13) 0.0570(6) Uani 1 1 d . . . . .
H45A H 0.676323 0.036214 0.540419 0.068 Uiso 1 1 calc R . . . .
H45B H 0.606888 0.101487 0.572170 0.068 Uiso 1 1 calc R . . . .
C46 C 0.8358(2) 0.10759(17) 0.49050(12) 0.0531(6) Uani 1 1 d . . . . .
C47 C 0.5401(2) 0.72420(17) 0.15527(13) 0.0579(6) Uani 1 1 d . . . . .
C48 C 1.4095(2) 0.05610(19) 0.70158(15) 0.0613(7) Uani 1 1 d . . . . .
C49 C 0.0941(2) 0.65321(18) -0.00027(12) 0.0572(6) Uani 1 1 d . . . . .
H49A H 0.100287 0.629226 -0.034436 0.069 Uiso 1 1 calc R . . . .
H49B H 0.025034 0.704178 -0.013201 0.069 Uiso 1 1 calc R . . . .
C50 C 0.1933(2) 0.74891(17) 0.02755(13) 0.0574(6) Uani 1 1 d . . . . .
C51 C 0.2917(2) 0.77090(17) 0.03613(13) 0.0581(6) Uani 1 1 d . . . . .
H51 H 0.286723 0.814592 0.052615 0.070 Uiso 1 1 calc R . . . .
C52 C 0.3033(2) 0.64301(19) -0.01352(12) 0.0571(6) Uani 1 1 d . . . . .
H52 H 0.308006 0.599999 -0.030674 0.069 Uiso 1 1 calc R . . . .
C53 C 0.7211(2) 0.03241(19) 0.69157(13) 0.0576(6) Uani 1 1 d . . . . .
C54 C 0.5162(2) 0.43786(18) 0.41225(13) 0.0568(6) Uani 1 1 d . . . . .
H54 H 0.459557 0.456043 0.436990 0.068 Uiso 1 1 calc R . . . .
C55 C 0.8987(2) -0.12696(17) 0.70870(14) 0.0588(6) Uani 1 1 d . . . . .
C56 C 0.8631(3) -0.10612(18) 0.76714(13) 0.0602(7) Uani 1 1 d . . . . .
C57 C 0.4012(2) 0.66641(19) -0.00590(12) 0.0563(6) Uani 1 1 d . . . . .
C58 C 1.2992(3) 0.16759(19) 0.74063(13) 0.0617(7) Uani 1 1 d . . . . .
H58 H 1.264769 0.226474 0.734700 0.074 Uiso 1 1 calc R . . . .
C59 C 1.3503(3) 0.00386(19) 0.81376(13) 0.0629(7) Uani 1 1 d . . . . .
C60 C 0.7796(3) -0.0314(2) 0.75784(14) 0.0662(7) Uani 1 1 d . . . . .
H60 H 0.756986 -0.018742 0.794672 0.079 Uiso 1 1 calc R . . . .
C61 C 1.2327(3) -0.0926(2) 0.86909(13) 0.0677(8) Uani 1 1 d . . . . .
C62 C 1.0365(3) -0.14723(19) 0.84621(13) 0.0682(8) Uani 1 1 d . . . . .
C63 C 1.2427(3) -0.1589(2) 0.83966(15) 0.0718(8) Uani 1 1 d . . . . .
C64 C 1.4061(3) -0.0127(2) 0.76556(16) 0.0711(8) Uani 1 1 d . . . . .
H64 H 1.445411 -0.071332 0.772806 0.085 Uiso 1 1 calc R . . . .
C65 C 1.2902(3) 0.0976(2) 0.80315(14) 0.0655(7) Uani 1 1 d . . . . .
C66 C 1.0263(3) -0.0800(2) 0.87482(14) 0.0757(9) Uani 1 1 d . . . . .
C67 C 1.1298(4) -0.0570(2) 0.88513(15) 0.0802(9) Uani 1 1 d . . . . .
H67 H 1.123480 -0.015326 0.903871 0.096 Uiso 1 1 calc R . . . .
C68 C 1.1393(3) -0.1835(2) 0.83091(15) 0.0729(8) Uani 1 1 d . . . . .
H68 H 1.146261 -0.226849 0.813764 0.087 Uiso 1 1 calc R . . . .
C69 C 0.7973(3) 0.4392(2) 0.15097(17) 0.0791(9) Uani 1 1 d . . . . .
H69A H 0.826104 0.478185 0.115416 0.119 Uiso 1 1 calc GR . . . .
H69B H 0.728197 0.433792 0.134220 0.119 Uiso 1 1 calc GR . . . .
H69C H 0.854490 0.381874 0.169608 0.119 Uiso 1 1 calc GR . . . .
C70 C 1.3387(3) -0.0675(2) 0.87721(14) 0.0767(9) Uani 1 1 d . . . . .
H70A H 1.406502 -0.119244 0.888834 0.092 Uiso 1 1 calc R . . . .
H70B H 1.333471 -0.046320 0.912920 0.092 Uiso 1 1 calc R . . . .
C71 C 0.1942(3) 0.3800(2) 0.03374(18) 0.0829(10) Uani 1 1 d D . . . .
H71A H 0.214581 0.374706 -0.007311 0.124 Uiso 1 1 calc GR . . . .
H71B H 0.126221 0.362534 0.044972 0.124 Uiso 1 1 calc GR . . . .
H71C H 0.256667 0.342268 0.068256 0.124 Uiso 1 1 calc GR . . . .
C72 C 0.9296(3) -0.1692(2) 0.83409(14) 0.0740(8) Uani 1 1 d . . . . .
H72A H 0.880671 -0.165698 0.868636 0.089 Uiso 1 1 calc R . . . .
H72B H 0.951305 -0.229382 0.836078 0.089 Uiso 1 1 calc R . . . .
C73 C -0.0667(4) 0.6562(2) 0.21742(19) 0.0871(11) Uani 1 1 d . . . . .
H73A H -0.128038 0.684373 0.181460 0.131 Uiso 1 1 calc GR . . . .
H73B H -0.007751 0.684618 0.206627 0.131 Uiso 1 1 calc GR . . . .
H73C H -0.096429 0.661186 0.256960 0.131 Uiso 1 1 calc GR . . . .
C74 C 0.5082(3) 0.5980(2) -0.07461(17) 0.0823(9) Uani 1 1 d . . . . .
H74A H 0.460304 0.645911 -0.112634 0.123 Uiso 1 1 calc GR . . . .
H74B H 0.479076 0.548441 -0.062341 0.123 Uiso 1 1 calc GR . . . .
H74C H 0.585805 0.580936 -0.085151 0.123 Uiso 1 1 calc GR . . . .
C75 C 0.6937(3) 0.2306(2) 0.31795(18) 0.0860(10) Uani 1 1 d . . . . .
H75A H 0.656651 0.279425 0.277360 0.129 Uiso 1 1 calc GR . . . .
H75B H 0.684730 0.177066 0.316903 0.129 Uiso 1 1 calc GR . . . .
H75C H 0.774336 0.224551 0.322817 0.129 Uiso 1 1 calc GR . . . .
C76 C 0.1680(3) 0.5020(2) 0.4285(2) 0.0904(11) Uani 1 1 d . . . . .
H76A H 0.165736 0.543352 0.384089 0.136 Uiso 1 1 calc GR . . . .
H76B H 0.184864 0.525745 0.459539 0.136 Uiso 1 1 calc GR . . . .
H76C H 0.094409 0.491919 0.434370 0.136 Uiso 1 1 calc GR . . . .
C77 C 0.3707(3) 0.2015(3) 0.2561(2) 0.0963(12) Uani 1 1 d . . . . .
H77A H 0.359000 0.183547 0.220486 0.144 Uiso 1 1 calc GR . . . .
H77B H 0.401410 0.149920 0.296136 0.144 Uiso 1 1 calc GR . . . .
H77C H 0.424136 0.234997 0.245342 0.144 Uiso 1 1 calc GR . . . .
C78 C 1.3071(4) 0.1097(4) 1.0398(2) 0.1075(13) Uani 1 1 d . . . . .
C79 C 0.0785(4) 0.8516(3) 0.0711(2) 0.1046(13) Uani 1 1 d . . . . .
H79A H 0.100229 0.901123 0.041998 0.157 Uiso 1 1 calc GR . . . .
H79B H 0.129364 0.822992 0.111904 0.157 Uiso 1 1 calc GR . . . .
H79C H 0.000537 0.871986 0.080176 0.157 Uiso 1 1 calc GR . . . .
C80 C 0.4062(4) 0.8279(3) 0.1899(2) 0.1093(15) Uani 1 1 d . . . . .
H80A H 0.337807 0.877826 0.171055 0.164 Uiso 1 1 calc GR . . . .
H80B H 0.457608 0.842081 0.214324 0.164 Uiso 1 1 calc GR . . . .
H80C H 0.385577 0.777844 0.219139 0.164 Uiso 1 1 calc GR . . . .
C81 C 0.9408(5) -0.0737(4) 0.3255(3) 0.1317(19) Uani 1 1 d . . . . .
C82 C 0.3146(5) 0.5854(4) 0.2124(3) 0.1224(16) Uani 1 1 d . . . . .
O21 O 1.3355(4) 0.1193(4) 1.0874(2) 0.200(2) Uani 1 1 d . . . . .
C83 C 0.4535(4) 0.6173(3) 0.3986(3) 0.1110(15) Uani 1 1 d . . . . .
H83A H 0.390212 0.609639 0.377907 0.166 Uiso 1 1 calc GR . . . .
H83B H 0.442478 0.679459 0.386010 0.166 Uiso 1 1 calc GR . . . .
H83C H 0.456957 0.589623 0.445979 0.166 Uiso 1 1 calc GR . . . .
C84 C 1.2240(4) 0.1805(3) 0.9867(3) 0.1216(15) Uani 1 1 d . . . . .
H84A H 1.155134 0.164647 0.984323 0.182 Uiso 1 1 calc GR . . . .
H84B H 1.256134 0.189961 0.945362 0.182 Uiso 1 1 calc GR . . . .
H84C H 1.205513 0.233884 0.995019 0.182 Uiso 1 1 calc GR . . . .
C85 C 0.9012(6) -0.0266(4) 0.3632(3) 0.156(2) Uani 1 1 d D . . . .
H85A H 0.858654 0.033249 0.335019 0.234 Uiso 1 1 calc GR . . . .
H85B H 0.965181 -0.026697 0.388793 0.234 Uiso 1 1 calc GR . . . .
H85C H 0.851510 -0.052959 0.392509 0.234 Uiso 1 1 calc GR . . . .
O22 O 0.2571(12) 0.6623(5) 0.1903(4) 0.328(6) Uani 1 1 d . . . . .
H22 H 0.253384 0.682154 0.149729 0.492 Uiso 1 1 calc GR . . . .
C87 C 0.3696(9) 0.5262(7) 0.1785(5) 0.246(5) Uani 1 1 d . . . . .
H87A H 0.311001 0.515529 0.156297 0.369 Uiso 1 1 calc GR . . . .
H87B H 0.418317 0.470950 0.210633 0.369 Uiso 1 1 calc GR . . . .
H87C H 0.415247 0.553657 0.146666 0.369 Uiso 1 1 calc GR . . . .
O23 O 0.8780(7) -0.0570(8) 0.2767(5) 0.423(8) Uani 1 1 d D . . . .
O24 O 1.3453(14) 0.0264(5) 1.0310(5) 0.400(7) Uani 1 1 d . . . . .
H24 H 1.377690 -0.013641 1.066354 0.600 Uiso 1 1 calc GR . . . .
O25 O 0.3132(12) 0.5568(7) 0.2754(4) 0.397(7) Uani 1 1 d . . . . .
C88 C 1.0216(10) -0.1848(10) 0.3007(8) 0.351(9) Uani 1 1 d D . . . .
H88 H 0.957437 -0.194652 0.285693 0.422 Uiso 1 1 calc R . . . .
O26 O 1.0261(6) -0.1321(5) 0.3397(4) 0.324(6) Uani 1 1 d D . . . .
C89 C 1.1349(9) -0.2161(8) 0.2918(6) 0.268(6) Uani 1 1 d D . . . .
H89A H 1.155936 -0.169739 0.257969 0.402 Uiso 1 1 calc GR . . . .
H89B H 1.145002 -0.265090 0.278527 0.402 Uiso 1 1 calc GR . . . .
H89C H 1.183142 -0.235309 0.332604 0.402 Uiso 1 1 calc GR . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C13 O1 C69 118.9(2) . . ?
C29 O2 C73 118.1(2) . . ?
C12 O3 C77 118.2(2) . . ?
C21 O4 C75 117.3(2) . . ?
C15 O5 C71 116.8(2) . . ?
C14 O6 C76 118.5(2) . . ?
C33 O11 C83 118.8(2) . . ?
C57 O13 C74 117.6(2) . . ?
C50 O16 C79 118.5(3) . . ?
C47 O17 C80 118.3(2) . . ?
C12 C1 C10 120.9(2) . . ?
C16 C1 C10 121.1(2) . . ?
C16 C1 C12 118.0(2) . . ?
C14 C2 C36 121.3(2) . . ?
C17 C2 C14 117.4(2) . . ?
C17 C2 C36 121.2(2) . . ?
C9 C3 C15 121.8(2) . . ?
C39 C4 C45 123.3(2) . . ?
C39 C4 C53 118.9(2) . . ?
C53 C4 C45 117.8(2) . . ?
C26 C5 C31 121.1(2) . . ?
C26 C5 C33 117.9(2) . . ?
C33 C5 C31 121.0(2) . . ?
C27 C6 C35 124.4(2) . . ?
C27 C6 C38 118.7(2) . . ?
C38 C6 C35 116.9(2) . . ?
C13 C7 C31 120.9(2) . . ?
C13 C7 C41 119.1(2) . . ?
C41 C7 C31 119.9(2) . . ?
C20 C8 C44 120.0(2) . . ?
C47 C8 C20 118.3(2) . . ?
C47 C8 C44 121.7(2) . . ?
C3 C9 C10 121.2(2) . . ?
C3 C9 C29 118.0(2) . . ?
C29 C9 C10 120.9(2) . . ?
C9 C10 C1 113.04(19) . . ?
C18 C11 C37 117.7(2) . . ?
C42 C11 C18 118.6(2) . . ?
C42 C11 C37 123.7(2) . . ?
O3 C12 C1 115.8(2) . . ?
O3 C12 C17 124.0(2) . . ?
C17 C12 C1 120.2(2) . . ?
O1 C13 C7 116.5(2) . . ?
O1 C13 C20 123.4(2) . . ?
C7 C13 C20 120.0(2) . . ?
O6 C14 C2 115.5(2) . . ?
O6 C14 C16 124.2(2) . . ?
C16 C14 C2 120.3(2) . . ?
O5 C15 C3 123.5(2) . . ?
O5 C15 C24 116.5(2) . . ?
C24 C15 C3 120.1(2) . . ?
C1 C16 C14 121.9(2) . . ?
C12 C17 C2 122.2(2) . . ?
O9 C18 C11 121.4(2) . . ?
O9 C18 C27 120.6(2) . . ?
C27 C18 C11 118.1(2) . . ?
C28 C19 C37 117.4(2) . . ?
C43 C19 C28 118.9(2) . . ?
C43 C19 C37 123.7(2) . . ?
C13 C20 C8 121.2(2) . . ?
O4 C21 C25 115.8(2) . . ?
C26 C21 O4 123.6(2) . . ?
C26 C21 C25 120.6(2) . . ?
C50 C22 C49 121.0(2) . . ?
C50 C22 C52 118.2(2) . . ?
C52 C22 C49 120.7(3) . . ?
C32 C23 C45 124.3(2) . . ?
C32 C23 C46 118.5(2) . . ?
C46 C23 C45 117.2(2) . . ?
C15 C24 C49 121.4(2) . . ?
C40 C24 C15 117.9(2) . . ?
C40 C24 C49 120.7(2) . . ?
C21 C25 C36 121.7(2) . . ?
C54 C25 C21 117.5(2) . . ?
C54 C25 C36 120.7(2) . . ?
C21 C26 C5 121.8(2) . . ?
C6 C27 C18 123.2(2) . . ?
O7 C28 C19 121.5(2) . . ?
O7 C28 C32 120.7(2) . . ?
C32 C28 C19 117.8(2) . . ?
O2 C29 C9 115.6(2) . . ?
O2 C29 C40 124.2(2) . . ?
C40 C29 C9 120.2(2) . . ?
C51 C30 C44 120.1(3) . . ?
C57 C30 C44 122.1(2) . . ?
C57 C30 C51 117.8(2) . . ?
C5 C31 C7 111.63(19) . . ?
C23 C32 C28 123.3(2) . . ?
O11 C33 C5 116.0(2) . . ?
O11 C33 C54 123.3(2) . . ?
C5 C33 C54 120.6(2) . . ?
C48 C34 C35 117.7(2) . . ?
C58 C34 C35 123.7(2) . . ?
C58 C34 C48 118.6(2) . . ?
C34 C35 C6 111.2(2) . . ?
C2 C36 C25 112.0(2) . . ?
C19 C37 C11 111.0(2) . . ?
O12 C38 C6 121.4(2) . . ?
O12 C38 C42 120.5(2) . . ?
C42 C38 C6 118.1(2) . . ?
C4 C39 C55 122.8(2) . . ?
C29 C40 C24 122.0(2) . . ?
C7 C41 C47 120.9(2) . . ?
C11 C42 C38 123.3(2) . . ?
C19 C43 C46 123.0(2) . . ?
C30 C44 C8 112.0(2) . . ?
C23 C45 C4 109.8(2) . . ?
O15 C46 C23 120.7(2) . . ?
O15 C46 C43 120.8(2) . . ?
C43 C46 C23 118.5(2) . . ?
O17 C47 C41 122.8(2) . . ?
C8 C47 O17 116.7(2) . . ?
C8 C47 C41 120.5(2) . . ?
O14 C48 C34 121.0(3) . . ?
O14 C48 C64 121.2(3) . . ?
C64 C48 C34 117.9(3) . . ?
C22 C49 C24 112.5(2) . . ?
O16 C50 C22 116.4(2) . . ?
O16 C50 C51 123.1(3) . . ?
C22 C50 C51 120.5(3) . . ?
C50 C51 C30 121.4(3) . . ?
C22 C52 C57 121.0(3) . . ?
O10 C53 C4 121.3(3) . . ?
O10 C53 C60 121.0(2) . . ?
C60 C53 C4 117.7(2) . . ?
C25 C54 C33 121.6(2) . . ?
O8 C55 C39 120.6(3) . . ?
O8 C55 C56 121.4(3) . . ?
C39 C55 C56 118.0(2) . . ?
C55 C56 C72 117.5(3) . . ?
C60 C56 C55 118.8(2) . . ?
C60 C56 C72 123.5(3) . . ?
O13 C57 C52 122.2(3) . . ?
C30 C57 O13 116.7(2) . . ?
C30 C57 C52 121.0(3) . . ?
C34 C58 C65 122.9(3) . . ?
C64 C59 C65 118.2(3) . . ?
C64 C59 C70 123.6(3) . . ?
C65 C59 C70 118.0(3) . . ?
C56 C60 C53 122.8(3) . . ?
C63 C61 C70 117.6(3) . . ?
C67 C61 C63 118.2(3) . . ?
C67 C61 C70 124.2(3) . . ?
C66 C62 C72 118.4(3) . . ?
C68 C62 C66 118.1(3) . . ?
C68 C62 C72 123.5(3) . . ?
O19 C63 C61 120.9(3) . . ?
O19 C63 C68 120.8(3) . . ?
C68 C63 C61 118.2(3) . . ?
C59 C64 C48 123.9(3) . . ?
O18 C65 C58 120.7(3) . . ?
O18 C65 C59 121.0(3) . . ?
C58 C65 C59 118.3(3) . . ?
O20 C66 C62 120.6(3) . . ?
O20 C66 C67 120.9(3) . . ?
C67 C66 C62 118.5(3) . . ?
C61 C67 C66 123.5(3) . . ?
C62 C68 C63 123.5(3) . . ?
C61 C70 C59 110.4(2) . . ?
C62 C72 C56 111.2(2) . . ?
O21 C78 C84 121.6(6) . . ?
O21 C78 O24 123.9(7) . . ?
C84 C78 O24 114.4(6) . . ?
O23 C81 C85 116.5(7) . . ?
O26 C81 C85 124.2(6) . . ?
O26 C81 O23 119.0(6) . . ?
O22 C82 C87 130.7(7) . . ?
O22 C82 O25 106.8(8) . . ?
O25 C82 C87 122.1(8) . . ?
C89 C88 O26 103.1(5) . . ?
C81 O26 C88 108.3(7) . . ?
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
O1 C13 1.376(3) . ?
O1 C69 1.399(3) . ?
O2 C29 1.375(3) . ?
O2 C73 1.405(3) . ?
O3 C12 1.379(3) . ?
O3 C77 1.404(3) . ?
O4 C21 1.384(3) . ?
O4 C75 1.407(4) . ?
O5 C15 1.370(3) . ?
O5 C71 1.459(3) . ?
O6 C14 1.377(3) . ?
O6 C76 1.416(4) . ?
O7 C28 1.215(3) . ?
O8 C55 1.224(3) . ?
O9 C18 1.216(3) . ?
O10 C53 1.216(3) . ?
O11 C33 1.375(3) . ?
O11 C83 1.410(4) . ?
O12 C38 1.224(3) . ?
O13 C57 1.385(3) . ?
O13 C74 1.415(4) . ?
O14 C48 1.214(3) . ?
O15 C46 1.215(3) . ?
O16 C50 1.379(3) . ?
O16 C79 1.414(4) . ?
O17 C47 1.382(3) . ?
O17 C80 1.397(4) . ?
C1 C10 1.516(3) . ?
C1 C12 1.395(3) . ?
C1 C16 1.383(3) . ?
O18 C65 1.223(4) . ?
O19 C63 1.220(4) . ?
C2 C14 1.397(3) . ?
C2 C17 1.390(3) . ?
C2 C36 1.508(3) . ?
C3 C9 1.386(3) . ?
C3 C15 1.394(3) . ?
C4 C39 1.328(4) . ?
C4 C45 1.511(4) . ?
C4 C53 1.485(3) . ?
C5 C26 1.386(4) . ?
C5 C31 1.518(3) . ?
C5 C33 1.388(3) . ?
C6 C27 1.327(3) . ?
C6 C35 1.509(3) . ?
C6 C38 1.484(4) . ?
C7 C13 1.382(3) . ?
C7 C31 1.531(3) . ?
C7 C41 1.382(3) . ?
C8 C20 1.397(4) . ?
C8 C44 1.523(3) . ?
C8 C47 1.381(4) . ?
C9 C10 1.510(3) . ?
C9 C29 1.395(3) . ?
C11 C18 1.483(4) . ?
C11 C37 1.510(4) . ?
C11 C42 1.330(4) . ?
C12 C17 1.380(3) . ?
C13 C20 1.388(3) . ?
C14 C16 1.386(3) . ?
C15 C24 1.392(4) . ?
C18 C27 1.474(4) . ?
C19 C28 1.486(3) . ?
C19 C37 1.506(3) . ?
C19 C43 1.328(4) . ?
C21 C25 1.400(3) . ?
C21 C26 1.382(3) . ?
C22 C49 1.517(4) . ?
C22 C50 1.387(4) . ?
C22 C52 1.390(4) . ?
C23 C32 1.325(4) . ?
C23 C45 1.508(3) . ?
C23 C46 1.488(3) . ?
C24 C40 1.390(4) . ?
C24 C49 1.520(3) . ?
C25 C36 1.509(3) . ?
C25 C54 1.387(4) . ?
C28 C32 1.477(4) . ?
C29 C40 1.385(3) . ?
C30 C44 1.509(4) . ?
C30 C51 1.393(4) . ?
C30 C57 1.383(4) . ?
O20 C66 1.222(4) . ?
C33 C54 1.391(4) . ?
C34 C35 1.502(4) . ?
C34 C48 1.487(4) . ?
C34 C58 1.334(4) . ?
C38 C42 1.470(4) . ?
C39 C55 1.467(4) . ?
C41 C47 1.395(4) . ?
C43 C46 1.463(4) . ?
C48 C64 1.465(4) . ?
C50 C51 1.388(4) . ?
C52 C57 1.391(4) . ?
C53 C60 1.475(4) . ?
C55 C56 1.481(4) . ?
C56 C60 1.328(4) . ?
C56 C72 1.513(4) . ?
C58 C65 1.474(4) . ?
C59 C64 1.327(4) . ?
C59 C65 1.485(4) . ?
C59 C70 1.508(4) . ?
C61 C63 1.474(4) . ?
C61 C67 1.333(5) . ?
C61 C70 1.503(5) . ?
C62 C66 1.477(5) . ?
C62 C68 1.330(5) . ?
C62 C72 1.504(5) . ?
C63 C68 1.473(5) . ?
C66 C67 1.466(5) . ?
C78 O21 1.180(6) . ?
C78 C84 1.446(7) . ?
C78 O24 1.450(9) . ?
C81 C85 1.351(7) . ?
C81 O23 1.206(7) . ?
C81 O26 1.159(6) . ?
C82 O22 1.203(8) . ?
C82 C87 1.479(9) . ?
C82 O25 1.280(9) . ?
C88 O26 1.462(4) . ?
C88 C89 1.372(5) . ?
