#------------------------------------------------------------------------------
#$Date: 2020-04-10 02:02:53 +0300 (Fri, 10 Apr 2020) $
#$Revision: 250568 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/46/4134660.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_4134660
loop_
_publ_author_name
'Chen, Xu-Lang'
'Shen, Yun-Jia'
'Gao, Chao'
'Yang, Jian'
'Sun, Xin'
'Zhang, Xin'
'Yang, Yu-Dong'
'Wei, Gong-Ping'
'Xiang, Jun-Feng'
'Sessler, Jonathan L.'
'Gong, Han-Yuan'
_publ_section_title
;
 Regulating the Structures of Self-Assembled Mechanically Interlocked
 Moleculecular Constructs via Dianion Precursor Substituent Effects.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b13473
_journal_year                    2020
_chemical_formula_sum            'C78 H68 N10 O29'
_chemical_formula_weight         1609.42
_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   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                96.260(18)
_cell_angle_beta                 90.40(2)
_cell_angle_gamma                107.24(3)
_cell_formula_units_Z            1
_cell_length_a                   8.155(3)
_cell_length_b                   13.187(3)
_cell_length_c                   17.132(3)
_cell_measurement_reflns_used    5547
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      62.500
_cell_measurement_theta_min      4.136
_cell_volume                     1747.6(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 5.3127
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1130
_diffrn_reflns_av_unetI/netI     0.1379
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9977
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        62.500
_diffrn_reflns_theta_max         62.500
_diffrn_reflns_theta_min         4.136
_exptl_absorpt_coefficient_mu    1.007
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78385
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       Prism
_exptl_crystal_F_000             838
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         5547
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1273
_refine_ls_R_factor_gt           0.0784
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0500P)²+2.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1781
_refine_ls_wR_factor_ref         0.2175
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3384
_reflns_number_total             5547
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b13473_si_006.cif
_cod_data_source_block           c
_cod_original_cell_volume        1747.6(8)
_cod_database_code               4134660
_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.
;
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
N1 N 0.8922(6) 0.2325(3) 0.7470(2) 0.0340(10) Uani 1 1 d . . . . .
N2 N 0.8687(5) 0.2379(3) 0.6223(2) 0.0320(9) Uani 1 1 d . . . . .
N3 N 0.7810(5) 0.2469(3) 0.4954(2) 0.0292(9) Uani 1 1 d . . . . .
H3C H 0.701462 0.270798 0.515474 0.035 Uiso 1 1 calc R U . . .
N4 N 0.6702(5) 0.2578(3) 0.3731(2) 0.0281(9) Uani 1 1 d . . . . .
N5 N 0.5189(5) 0.2717(3) 0.2738(2) 0.0318(9) Uani 1 1 d . . . . .
C1 C 0.9439(7) 0.2018(4) 0.8218(3) 0.0351(11) Uani 1 1 d . . . . .
H1A H 0.914260 0.244729 0.865986 0.042 Uiso 1 1 calc R U . . .
H1B H 1.067173 0.213759 0.824590 0.042 Uiso 1 1 calc R U . . .
C2 C 0.9681(7) 0.2207(4) 0.6799(3) 0.0322(11) Uani 1 1 d . . . . .
H2A H 1.070445 0.203687 0.673568 0.039 Uiso 1 1 calc R U . . .
C3 C 0.7411(7) 0.2556(4) 0.7323(3) 0.0386(12) Uani 1 1 d . . . . .
H3A H 0.663212 0.265822 0.769424 0.046 Uiso 1 1 calc R U . . .
C4 C 0.7266(7) 0.2606(4) 0.6546(3) 0.0355(12) Uani 1 1 d . . . . .
H4A H 0.638809 0.276199 0.627965 0.043 Uiso 1 1 calc R U . . .
C5 C 0.8945(6) 0.2231(4) 0.5399(3) 0.0300(11) Uani 1 1 d . . . . .
C6 C 1.0241(7) 0.1845(5) 0.5116(3) 0.0393(13) Uani 1 1 d . . . . .
H6A H 1.100847 0.169005 0.545383 0.047 Uiso 1 1 calc R U . . .
C7 C 1.0360(7) 0.1696(5) 0.4310(3) 0.0443(14) Uani 1 1 d . . . . .
H7A H 1.121448 0.143133 0.409347 0.053 Uiso 1 1 calc R U . . .
C8 C 0.9204(7) 0.1943(5) 0.3827(3) 0.0390(12) Uani 1 1 d . . . . .
H8A H 0.926497 0.185728 0.328258 0.047 Uiso 1 1 calc R U . . .
C9 C 0.7959(6) 0.2321(4) 0.4181(3) 0.0283(10) Uani 1 1 d . . . . .
C10 C 0.6484(6) 0.2408(4) 0.2946(3) 0.0308(11) Uani 1 1 d . . . . .
H10A H 0.715225 0.211558 0.260552 0.037 Uiso 1 1 calc R U . . .
C11 C 0.5433(6) 0.3001(4) 0.4027(3) 0.0331(11) Uani 1 1 d . . . . .
H11A H 0.527089 0.318770 0.455361 0.040 Uiso 1 1 calc R U . . .
C12 C 0.4489(6) 0.3091(4) 0.3414(3) 0.0325(11) Uani 1 1 d . . . . .
H12A H 0.354700 0.335179 0.343184 0.039 Uiso 1 1 calc R U . . .
C13 C 0.4348(6) 0.2475(4) 0.1939(3) 0.0344(11) Uani 1 1 d . . . . .
H13A H 0.520943 0.261852 0.154535 0.041 Uiso 1 1 calc R U . . .
H13B H 0.360775 0.292184 0.188564 0.041 Uiso 1 1 calc R U . . .
C14 C 0.3306(6) 0.1316(4) 0.1826(3) 0.0292(11) Uani 1 1 d . . . . .
C15 C 0.3739(6) 0.0564(4) 0.1296(3) 0.0310(11) Uani 1 1 d . . . . .
H15A H 0.464088 0.078495 0.096385 0.037 Uiso 1 1 calc R U . . .
C16 C 0.2835(6) -0.0505(4) 0.1264(3) 0.0285(11) Uani 1 1 d . . . . .
H16A H 0.313524 -0.100102 0.091061 0.034 Uiso 1 1 calc R U . . .
C17 C 0.1494(6) -0.0848(4) 0.1750(3) 0.0310(11) Uani 1 1 d . . . . .
C18 C 0.1023(6) -0.0096(4) 0.2268(3) 0.0311(11) Uani 1 1 d . . . . .
H18A H 0.010385 -0.031654 0.259134 0.037 Uiso 1 1 calc R U . . .
C19 C 0.1929(6) 0.0976(4) 0.2298(3) 0.0319(11) Uani 1 1 d . . . . .
H19A H 0.160779 0.147442 0.264006 0.038 Uiso 1 1 calc R U . . .
C20 C 0.6476(6) -0.0491(4) 0.3515(3) 0.0316(11) Uani 1 1 d . . . . .
C21 C 0.6431(7) -0.0355(4) 0.4982(3) 0.0333(11) Uani 1 1 d . . . . .
H21A H 0.740154 -0.058828 0.496827 0.040 Uiso 1 1 calc R U . . .
C22 C 0.5684(6) -0.0232(4) 0.4290(3) 0.0291(11) Uani 1 1 d . . . . .
C23 C 0.4249(6) 0.0133(4) 0.4295(3) 0.0306(11) Uani 1 1 d . . . . .
C24 C 0.1497(7) 0.5563(5) 0.8926(3) 0.0380(12) Uani 1 1 d . . . . .
C25 C 0.2369(7) 0.5625(4) 0.9703(3) 0.0350(12) Uani 1 1 d . . . . .
C26 C 0.3258(7) 0.6614(4) 1.0090(3) 0.0323(11) Uani 1 1 d . . . . .
C27 C 0.4263(7) 0.6708(4) 1.0773(3) 0.0338(11) Uani 1 1 d . . . . .
H27A H 0.489724 0.737787 1.101439 0.041 Uiso 1 1 calc R U . . .
C28 C 0.4302(7) 0.5781(4) 1.1086(3) 0.0351(12) Uani 1 1 d . . . . .
C29 C 0.3363(7) 0.4781(4) 1.0719(3) 0.0411(13) Uani 1 1 d . . . . .
H29A H 0.338151 0.416786 1.093636 0.049 Uiso 1 1 calc R U . . .
C30 C 0.2401(7) 0.4692(5) 1.0033(3) 0.0394(12) Uani 1 1 d . . . . .
H30A H 0.177811 0.402094 0.978908 0.047 Uiso 1 1 calc R U . . .
C31 C 0.5444(7) 0.5932(4) 1.1808(3) 0.0379(12) Uani 1 1 d . . . . .
C32 C 0.8045(6) 0.0353(5) 0.1347(3) 0.0333(12) Uani 1 1 d . . . . .
C33 C 0.9022(6) 0.0154(4) 0.0636(3) 0.0328(12) Uani 1 1 d . . . . .
C34 C 0.8823(7) -0.0855(5) 0.0280(3) 0.0354(12) Uani 1 1 d D . . . .
C35 C 0.9793(7) -0.1044(5) -0.0362(3) 0.0346(12) Uani 1 1 d . . . . .
C36 C 0.1133(7) 0.4812(4) 0.6582(3) 0.0418(14) Uani 1 1 d . . . . .
C37 C 0.0519(7) 0.4906(4) 0.5763(3) 0.0369(12) Uani 1 1 d . . . . .
C38 C -0.0993(7) 0.5136(4) 0.5635(3) 0.0427(13) Uani 1 1 d . . . . .
C39 C -0.1556(8) 0.5233(4) 0.4876(3) 0.0421(14) Uani 1 1 d . . . . .
O1 O 0.7573(5) -0.0963(3) 0.3502(2) 0.0435(9) Uani 1 1 d . . . . .
O1W O 0.4125(10) 0.3227(8) 0.5873(4) 0.135(3) Uani 1 1 d D . . . .
H1WB H 0.488(14) 0.386(6) 0.568(8) 0.203 Uiso 1 1 d D U . . .
H1WA H 0.338(13) 0.348(9) 0.623(6) 0.203 Uiso 1 1 d D U . . .
O2 O 0.5897(5) -0.0171(3) 0.2918(2) 0.0377(8) Uani 1 1 d . . . . .
O2W O -0.1044(7) 0.6716(5) 0.7588(4) 0.0872(19) Uani 1 1 d D . . . .
H2WB H -0.198(7) 0.606(4) 0.753(6) 0.131 Uiso 1 1 d D U . . .
H2WA H -0.009(7) 0.656(7) 0.784(6) 0.131 Uiso 1 1 d D U . . .
O3 O 0.3508(8) 0.0263(5) 0.3705(4) 0.0287(14) Uani 0.5 1 d . . P . .
H3B H 0.404435 0.015979 0.331659 0.043 Uiso 0.5 1 calc R U P . .
O4 O 0.0801(5) 0.4617(3) 0.8555(2) 0.0467(10) Uani 1 1 d . . . . .
H4B H 0.056150 0.466977 0.809881 0.070 Uiso 0.5 1 calc R U P . .
O5 O 0.1472(5) 0.6390(3) 0.8648(2) 0.0443(9) Uani 1 1 d . . . . .
O6 O 0.3251(6) 0.7562(3) 0.9827(2) 0.0538(11) Uani 1 1 d . . . . .
H6B H 0.270935 0.743772 0.940492 0.081 Uiso 1 1 calc R U . . .
O7 O 0.6214(5) 0.6809(3) 1.2142(2) 0.0496(10) Uani 1 1 d . . . . .
O8 O 0.5524(5) 0.5030(3) 1.2048(2) 0.0486(10) Uani 1 1 d . . . . .
H8B H 0.614299 0.516318 1.244805 0.073 Uiso 0.5 1 calc R U P . .
O9 O 0.8217(5) 0.1268(3) 0.1666(2) 0.0393(9) Uani 1 1 d . . . . .
O10 O 0.7083(5) -0.0510(3) 0.16027(19) 0.0379(9) Uani 1 1 d . . . . .
H10B H 0.672948 -0.035589 0.203282 0.057 Uiso 0.5 1 calc R U P . .
O11 O 0.9463(13) -0.2021(8) -0.0678(6) 0.025(2) Uani 0.3 1 d . . P A 1
H11C H 1.007313 -0.204596 -0.105365 0.037 Uiso 0.3 1 calc R U P A 1
O11A O 0.7928(19) -0.1668(10) 0.0521(9) 0.032(4) Uani 0.2 1 d D . P B 2
H11D H 0.744821 -0.150973 0.091413 0.047 Uiso 0.2 1 calc R U P B 2
O12 O 0.2527(5) 0.4638(3) 0.6674(2) 0.0495(10) Uani 1 1 d . . . . .
O13 O 0.0108(6) 0.4869(4) 0.7135(2) 0.0524(11) Uani 1 1 d . . . . .
H13C H -0.073125 0.500677 0.696062 0.079 Uiso 0.5 1 calc R U P . .
O14 O -0.2046(15) 0.5293(9) 0.6190(6) 0.035(3) Uani 0.3 1 d . . P C 1
H14A H -0.167565 0.520865 0.661658 0.052 Uiso 0.3 1 calc R U P C 1
O14A O -0.302(3) 0.5475(17) 0.4861(13) 0.061(6) Uani 0.2 1 d . . P D 2
H14C H -0.329474 0.551166 0.440597 0.092 Uiso 0.2 1 calc R U P D 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 N1 C3 109.3(4) . . ?
C2 N1 C1 123.6(4) . . ?
C3 N1 C1 125.8(4) . . ?
C2 N2 C4 109.5(4) . . ?
C2 N2 C5 125.6(4) . . ?
C4 N2 C5 124.6(4) . . ?
C5 N3 C9 116.8(4) . . ?
C5 N3 H3C 121.6 . . ?
C9 N3 H3C 121.6 . . ?
C10 N4 C11 108.1(4) . . ?
C10 N4 C9 125.8(4) . . ?
C11 N4 C9 126.0(4) . . ?
C10 N5 C12 108.8(4) . . ?
C10 N5 C13 124.8(4) . . ?
C12 N5 C13 124.9(4) . . ?
N1 C1 C17 108.2(4) . 2_656 ?
N1 C1 H1A 110.1 . . ?
C17 C1 H1A 110.1 2_656 . ?
N1 C1 H1B 110.1 . . ?
C17 C1 H1B 110.1 2_656 . ?
H1A C1 H1B 108.4 . . ?
N1 C2 N2 107.1(4) . . ?
N1 C2 H2A 126.4 . . ?
N2 C2 H2A 126.4 . . ?
C4 C3 N1 107.9(5) . . ?
C4 C3 H3A 126.0 . . ?
N1 C3 H3A 126.0 . . ?
C3 C4 N2 106.1(4) . . ?
C3 C4 H4A 127.0 . . ?
N2 C4 H4A 127.0 . . ?
N3 C5 C6 124.6(5) . . ?
N3 C5 N2 114.1(4) . . ?
C6 C5 N2 121.3(4) . . ?
C5 C6 C7 117.3(5) . . ?
C5 C6 H6A 121.3 . . ?
C7 C6 H6A 121.3 . . ?
C8 C7 C6 119.7(5) . . ?
C8 C7 H7A 120.1 . . ?
C6 C7 H7A 120.1 . . ?
C9 C8 C7 117.4(5) . . ?
C9 C8 H8A 121.3 . . ?
C7 C8 H8A 121.3 . . ?
N3 C9 C8 124.2(4) . . ?
N3 C9 N4 114.5(4) . . ?
C8 C9 N4 121.2(4) . . ?
N5 C10 N4 109.0(4) . . ?
N5 C10 H10A 125.5 . . ?
N4 C10 H10A 125.5 . . ?
C12 C11 N4 107.1(4) . . ?
C12 C11 H11A 126.4 . . ?
N4 C11 H11A 126.4 . . ?
C11 C12 N5 106.9(4) . . ?
C11 C12 H12A 126.5 . . ?
N5 C12 H12A 126.5 . . ?
N5 C13 C14 108.3(4) . . ?
N5 C13 H13A 110.0 . . ?
C14 C13 H13A 110.0 . . ?
N5 C13 H13B 110.0 . . ?
C14 C13 H13B 110.0 . . ?
H13A C13 H13B 108.4 . . ?
C19 C14 C15 119.0(5) . . ?
C19 C14 C13 118.4(5) . . ?
C15 C14 C13 122.5(4) . . ?
C16 C15 C14 120.2(4) . . ?
C16 C15 H15A 119.9 . . ?
C14 C15 H15A 119.9 . . ?
C17 C16 C15 120.8(5) . . ?
C17 C16 H16A 119.6 . . ?
C15 C16 H16A 119.6 . . ?
C16 C17 C18 119.3(5) . . ?
C16 C17 C1 122.5(5) . 2_656 ?
C18 C17 C1 118.0(4) . 2_656 ?
C19 C18 C17 119.8(5) . . ?
C19 C18 H18A 120.1 . . ?
C17 C18 H18A 120.1 . . ?
C14 C19 C18 120.8(5) . . ?
C14 C19 H19A 119.6 . . ?
C18 C19 H19A 119.6 . . ?
O1 C20 O2 125.7(4) . . ?
O1 C20 C22 120.2(4) . . ?
O2 C20 C22 114.1(4) . . ?
C22 C21 C23 120.9(5) . 2_656 ?
C22 C21 H21A 119.6 . . ?
C23 C21 H21A 119.6 2_656 . ?
C21 C22 C23 120.7(5) . . ?
C21 C22 C20 118.7(4) . . ?
C23 C22 C20 120.6(4) . . ?
O3 C23 C22 124.7(5) . . ?
O3 C23 C21 116.9(5) . 2_656 ?
C22 C23 C21 118.4(5) . 2_656 ?
O5 C24 O4 122.4(5) . . ?
O5 C24 C25 120.6(5) . . ?
O4 C24 C25 117.0(5) . . ?
C26 C25 C30 119.1(5) . . ?
C26 C25 C24 119.3(5) . . ?
C30 C25 C24 121.5(5) . . ?
O6 C26 C25 123.1(5) . . ?
O6 C26 C27 115.6(5) . . ?
C25 C26 C27 121.3(5) . . ?
C26 C27 C28 118.9(5) . . ?
C26 C27 H27A 120.5 . . ?
C28 C27 H27A 120.5 . . ?
C29 C28 C27 120.4(5) . . ?
C29 C28 C31 123.1(5) . . ?
C27 C28 C31 116.5(5) . . ?
C30 C29 C28 120.4(5) . . ?
C30 C29 H29A 119.8 . . ?
C28 C29 H29A 119.8 . . ?
C29 C30 C25 119.8(5) . . ?
C29 C30 H30A 120.1 . . ?
C25 C30 H30A 120.1 . . ?
O7 C31 O8 123.2(5) . . ?
O7 C31 C28 122.8(5) . . ?
O8 C31 C28 114.0(5) . . ?
O9 C32 O10 124.2(4) . . ?
O9 C32 C33 121.6(5) . . ?
O10 C32 C33 114.2(5) . . ?
C34 C33 C35 120.6(5) . 2_755 ?
C34 C33 C32 121.6(5) . . ?
C35 C33 C32 117.7(5) 2_755 . ?
O11A C34 C33 124.3(9) . . ?
O11A C34 C35 113.8(9) . . ?
C33 C34 C35 121.6(5) . . ?
O11 C35 C34 116.9(6) . . ?
O11 C35 C33 125.2(6) . 2_755 ?
C34 C35 C33 117.8(5) . 2_755 ?
O12 C36 O13 124.0(5) . . ?
O12 C36 C37 119.4(6) . . ?
O13 C36 C37 116.5(5) . . ?
C38 C37 C39 120.0(5) . 2_566 ?
C38 C37 C36 121.5(5) . . ?
C39 C37 C36 118.4(5) 2_566 . ?
O14 C38 C37 125.0(7) . . ?
O14 C38 C39 113.5(7) . . ?
C37 C38 C39 121.5(6) . . ?
O14A C39 C38 113.6(11) . . ?
C38 C39 C37 118.4(5) . 2_566 ?
H1WB O1W H1WA 106.1(16) . . ?
H2WB O2W H2WA 106.6(16) . . ?
C23 O3 H3B 109.5 . . ?
C24 O4 H4B 109.5 . . ?
C26 O6 H6B 109.5 . . ?
C31 O8 H8B 109.5 . . ?
C32 O10 H10B 109.5 . . ?
C35 O11 H11C 109.5 . . ?
C34 O11A H11D 109.5 . . ?
C36 O13 H13C 109.5 . . ?
C38 O14 H14A 109.5 . . ?
C39 O14A H14C 109.5 . . ?
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
N1 C2 1.327(7) . ?
N1 C3 1.382(7) . ?
N1 C1 1.480(6) . ?
N2 C2 1.353(6) . ?
N2 C4 1.385(7) . ?
N2 C5 1.430(6) . ?
N3 C5 1.323(6) . ?
N3 C9 1.328(6) . ?
N3 H3C 0.8600 . ?
N4 C10 1.340(6) . ?
N4 C11 1.389(7) . ?
N4 C9 1.419(6) . ?
N5 C10 1.301(6) . ?
N5 C12 1.401(7) . ?
N5 C13 1.485(7) . ?
C1 C17 1.512(7) 2_656 ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9300 . ?
C3 C4 1.346(8) . ?
C3 H3A 0.9300 . ?
C4 H4A 0.9300 . ?
C5 C6 1.372(7) . ?
C6 C7 1.382(8) . ?
C6 H6A 0.9300 . ?
C7 C8 1.382(8) . ?
C7 H7A 0.9300 . ?
C8 C9 1.374(7) . ?
C8 H8A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 C12 1.333(7) . ?
C11 H11A 0.9300 . ?
C12 H12A 0.9300 . ?
C13 C14 1.503(7) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C19 1.382(7) . ?
C14 C15 1.395(7) . ?
C15 C16 1.379(7) . ?
C15 H15A 0.9300 . ?
C16 C17 1.377(7) . ?
C16 H16A 0.9300 . ?
C17 C18 1.399(8) . ?
C18 C19 1.382(7) . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9300 . ?
C20 O1 1.232(6) . ?
C20 O2 1.286(6) . ?
C20 C22 1.530(7) . ?
C21 C22 1.376(7) . ?
C21 C23 1.399(7) 2_656 ?
C21 H21A 0.9300 . ?
C22 C23 1.390(7) . ?
C23 O3 1.227(8) . ?
C24 O5 1.242(7) . ?
C24 O4 1.297(7) . ?
C24 C25 1.488(8) . ?
C25 C26 1.383(8) . ?
C25 C30 1.416(7) . ?
C26 O6 1.375(6) . ?
C26 C27 1.396(7) . ?
C27 C28 1.397(7) . ?
C27 H27A 0.9300 . ?
C28 C29 1.391(8) . ?
C28 C31 1.502(7) . ?
C29 C30 1.383(8) . ?
C29 H29A 0.9300 . ?
C30 H30A 0.9300 . ?
C31 O7 1.217(7) . ?
C31 O8 1.319(7) . ?
C32 O9 1.237(7) . ?
C32 O10 1.299(6) . ?
C32 C33 1.501(7) . ?
C33 C34 1.364(8) . ?
C33 C35 1.410(7) 2_755 ?
C34 O11A 1.221(9) . ?
C34 C35 1.402(7) . ?
C35 O11 1.291(12) . ?
C36 O12 1.237(7) . ?
C36 O13 1.279(8) . ?
C36 C37 1.515(8) . ?
C37 C38 1.375(8) . ?
C37 C39 1.418(9) 2_566 ?
C38 O14 1.327(13) . ?
C38 C39 1.407(8) . ?
C39 O14A 1.33(3) . ?
O1W H1WB 0.970(11) . ?
O1W H1WA 0.965(11) . ?
O2W H2WB 0.967(11) . ?
O2W H2WA 0.966(11) . ?
O3 H3B 0.8200 . ?
O4 H4B 0.8200 . ?
O6 H6B 0.8200 . ?
O8 H8B 0.8200 . ?
O10 H10B 0.8200 . ?
O11 H11C 0.8200 . ?
O11A H11D 0.8200 . ?
O13 H13C 0.8200 . ?
O14 H14A 0.8200 . ?
O14A H14C 0.8200 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N1 C1 C17 -86.3(6) . . . 2_656 ?
C3 N1 C1 C17 79.4(6) . . . 2_656 ?
C3 N1 C2 N2 1.1(6) . . . . ?
C1 N1 C2 N2 168.9(4) . . . . ?
C4 N2 C2 N1 -0.3(6) . . . . ?
C5 N2 C2 N1 -173.6(4) . . . . ?
C2 N1 C3 C4 -1.6(6) . . . . ?
C1 N1 C3 C4 -169.0(5) . . . . ?
N1 C3 C4 N2 1.3(6) . . . . ?
C2 N2 C4 C3 -0.7(6) . . . . ?
C5 N2 C4 C3 172.7(5) . . . . ?
C9 N3 C5 C6 -0.2(7) . . . . ?
C9 N3 C5 N2 -178.3(4) . . . . ?
C2 N2 C5 N3 -179.1(5) . . . . ?
C4 N2 C5 N3 8.6(7) . . . . ?
C2 N2 C5 C6 2.7(8) . . . . ?
C4 N2 C5 C6 -169.6(5) . . . . ?
N3 C5 C6 C7 0.0(8) . . . . ?
N2 C5 C6 C7 178.0(5) . . . . ?
C5 C6 C7 C8 0.5(9) . . . . ?
C6 C7 C8 C9 -0.7(9) . . . . ?
C5 N3 C9 C8 -0.1(7) . . . . ?
C5 N3 C9 N4 179.4(4) . . . . ?
C7 C8 C9 N3 0.5(8) . . . . ?
C7 C8 C9 N4 -179.0(5) . . . . ?
C10 N4 C9 N3 -173.6(4) . . . . ?
C11 N4 C9 N3 3.1(7) . . . . ?
C10 N4 C9 C8 5.9(7) . . . . ?
C11 N4 C9 C8 -177.4(5) . . . . ?
C12 N5 C10 N4 -1.2(5) . . . . ?
C13 N5 C10 N4 -168.0(4) . . . . ?
C11 N4 C10 N5 1.2(5) . . . . ?
C9 N4 C10 N5 178.4(4) . . . . ?
C10 N4 C11 C12 -0.8(5) . . . . ?
C9 N4 C11 C12 -178.0(4) . . . . ?
N4 C11 C12 N5 0.1(5) . . . . ?
C10 N5 C12 C11 0.7(6) . . . . ?
C13 N5 C12 C11 167.5(4) . . . . ?
C10 N5 C13 C14 73.3(6) . . . . ?
C12 N5 C13 C14 -91.5(5) . . . . ?
N5 C13 C14 C19 64.3(5) . . . . ?
N5 C13 C14 C15 -111.8(5) . . . . ?
C19 C14 C15 C16 -2.0(7) . . . . ?
C13 C14 C15 C16 174.1(4) . . . . ?
C14 C15 C16 C17 0.2(7) . . . . ?
C15 C16 C17 C18 1.5(7) . . . . ?
C15 C16 C17 C1 -175.0(4) . . . 2_656 ?
C16 C17 C18 C19 -1.4(7) . . . . ?
C1 C17 C18 C19 175.3(4) 2_656 . . . ?
C15 C14 C19 C18 2.1(7) . . . . ?
C13 C14 C19 C18 -174.1(4) . . . . ?
C17 C18 C19 C14 -0.5(7) . . . . ?
C23 C21 C22 C23 1.1(8) 2_656 . . . ?
C23 C21 C22 C20 -179.7(5) 2_656 . . . ?
O1 C20 C22 C21 11.7(7) . . . . ?
O2 C20 C22 C21 -167.9(4) . . . . ?
O1 C20 C22 C23 -169.0(5) . . . . ?
O2 C20 C22 C23 11.3(7) . . . . ?
C21 C22 C23 O3 -179.8(6) . . . . ?
C20 C22 C23 O3 0.9(8) . . . . ?
C21 C22 C23 C21 -1.1(8) . . . 2_656 ?
C20 C22 C23 C21 179.7(4) . . . 2_656 ?
O5 C24 C25 C26 -4.5(8) . . . . ?
O4 C24 C25 C26 174.5(5) . . . . ?
O5 C24 C25 C30 179.5(5) . . . . ?
O4 C24 C25 C30 -1.5(8) . . . . ?
C30 C25 C26 O6 -177.7(5) . . . . ?
C24 C25 C26 O6 6.2(8) . . . . ?
C30 C25 C26 C27 3.8(8) . . . . ?
C24 C25 C26 C27 -172.3(5) . . . . ?
O6 C26 C27 C28 178.4(5) . . . . ?
C25 C26 C27 C28 -3.0(7) . . . . ?
C26 C27 C28 C29 0.5(8) . . . . ?
C26 C27 C28 C31 178.3(5) . . . . ?
C27 C28 C29 C30 1.0(8) . . . . ?
C31 C28 C29 C30 -176.7(5) . . . . ?
C28 C29 C30 C25 -0.1(8) . . . . ?
C26 C25 C30 C29 -2.2(8) . . . . ?
C24 C25 C30 C29 173.8(5) . . . . ?
C29 C28 C31 O7 -177.3(5) . . . . ?
C27 C28 C31 O7 5.0(8) . . . . ?
C29 C28 C31 O8 2.1(7) . . . . ?
C27 C28 C31 O8 -175.6(5) . . . . ?
O9 C32 C33 C34 -179.5(5) . . . . ?
O10 C32 C33 C34 3.1(7) . . . . ?
O9 C32 C33 C35 2.7(7) . . . 2_755 ?
O10 C32 C33 C35 -174.7(4) . . . 2_755 ?
C35 C33 C34 O11A 173.9(10) 2_755 . . . ?
C32 C33 C34 O11A -3.8(12) . . . . ?
C35 C33 C34 C35 0.7(8) 2_755 . . . ?
C32 C33 C34 C35 -177.1(4) . . . . ?
C33 C34 C35 O11 -177.3(6) . . . . ?
O11A C34 C35 C33 -174.5(9) . . . 2_755 ?
C33 C34 C35 C33 -0.7(8) . . . 2_755 ?
O12 C36 C37 C38 -177.7(5) . . . . ?
O13 C36 C37 C38 5.6(8) . . . . ?
O12 C36 C37 C39 1.4(8) . . . 2_566 ?
O13 C36 C37 C39 -175.4(5) . . . 2_566 ?
C39 C37 C38 O14 -179.2(8) 2_566 . . . ?
C36 C37 C38 O14 -0.1(10) . . . . ?
C39 C37 C38 C39 0.4(9) 2_566 . . . ?
C36 C37 C38 C39 179.4(5) . . . . ?
C37 C38 C39 O14A -178.8(11) . . . . ?
O14 C38 C39 C37 179.2(7) . . . 2_566 ?
C37 C38 C39 C37 -0.4(9) . . . 2_566 ?
