#------------------------------------------------------------------------------
#$Date: 2021-08-19 01:11:09 +0300 (Thu, 19 Aug 2021) $
#$Revision: 268125 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/43/1564370.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_1564370
loop_
_publ_author_name
'Weng, Guo-Guo'
'Hong, Ben-Kun'
'Bao, Song-Song'
'Wen, Yujie'
'Wu, Lan-Qing'
'Huang, Xin-Da'
'Jia, Jia-Ge'
'Wen, Ge-Hua'
'Li, Shuhua'
'Peng, Luming'
'Zheng, Li-Min'
_publ_section_title
;
 From helix to superhelix: hierarchical assembly of homochiral van der
 Waals 1D coordination polymers
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC01913A
_journal_year                    2021
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C27 H57 N3 O9 P3 Tb, C2 H4 O2, 2(H2 O)'
_chemical_formula_sum            'C29 H65 N3 O13 P3 Tb'
_chemical_formula_weight         915.67
_space_group_crystal_system      hexagonal
_space_group_IT_number           170
_space_group_name_Hall           'P 65'
_space_group_name_H-M_alt        'P 65'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-07-02 deposited with the CCDC.	2021-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   17.0143(5)
_cell_length_b                   17.0143(5)
_cell_length_c                   23.5290(10)
_cell_measurement_reflns_used    9966
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.475
_cell_measurement_theta_min      2.215
_cell_volume                     5898.8(4)
_computing_cell_refinement       'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_data_collection       'APEX 3'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 4K
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 with TXS'
_diffrn_measurement_method       CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            55509
_diffrn_reflns_point_group_measured_fraction_full 0.902
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.215
_exptl_absorpt_coefficient_mu    1.982
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.3540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_description       rod-like
_exptl_crystal_F_000             2844
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.978
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Flack x determined using 2983 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.010(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         7990
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0255
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0301P)²+4.0442P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0597
_reflns_Friedel_coverage         0.729
_reflns_Friedel_fraction_full    0.799
_reflns_Friedel_fraction_max     0.765
_reflns_number_gt                7514
_reflns_number_total             7990
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1sc01913a2.cif
_cod_data_source_block           2
_cod_database_code               1564370
_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.
;
_shelx_estimated_absorpt_t_min   0.637
_shelx_estimated_absorpt_t_max   0.826
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'-x, -y, z+1/2'
'y, -x+y, z+1/6'
'x-y, x, z+5/6'
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
Tb1 Tb 0.99935(2) 0.97242(2) 0.99896(2) 0.01369(6) Uani 1 1 d . . . . .
P1 P 0.87012(8) 1.03425(8) 1.04367(6) 0.0152(3) Uani 1 1 d . . . . .
P2 P 1.16880(8) 1.14050(8) 0.95279(6) 0.0149(2) Uani 1 1 d . . . . .
P3 P 1.09876(9) 0.86998(9) 0.91715(6) 0.0188(3) Uani 1 1 d . . . . .
O1 O 0.9126(2) 0.9905(2) 1.07975(16) 0.0172(8) Uani 1 1 d . . . . .
O2 O 0.9119(2) 1.0469(2) 0.98479(15) 0.0191(7) Uani 1 1 d . . . . .
O3 O 0.8735(2) 1.1171(2) 1.06899(16) 0.0193(8) Uani 1 1 d . . . . .
O4 O 1.1326(2) 1.1243(2) 1.01357(15) 0.0186(7) Uani 1 1 d . . . . .
O5 O 1.0926(2) 1.0648(2) 0.91842(16) 0.0181(8) Uani 1 1 d . . . . .
O6 O 1.2608(2) 1.1509(2) 0.94470(17) 0.0230(8) Uani 1 1 d . . . . .
O7 O 1.0836(3) 0.9096(3) 0.97119(16) 0.0253(8) Uani 1 1 d . . . . .
O8 O 1.0655(3) 0.8930(3) 0.86315(16) 0.0226(8) Uani 1 1 d . . . . .
O9 O 1.0615(3) 0.7691(3) 0.92438(18) 0.0281(9) Uani 1 1 d . . . . .
O10 O 1.1323(4) 0.6743(4) 0.9008(2) 0.0485(13) Uani 1 1 d G . . . .
H10C H 1.114377 0.714172 0.906793 0.073 Uiso 1 1 d G U . . .
O11 O 1.1755(4) 0.7429(4) 0.8184(2) 0.0669(17) Uani 1 1 d . . . . .
O1W O 1.3970(6) 1.2975(7) 0.8863(6) 0.138(4) Uani 1 1 d G . . . .
H1WA H 1.361668 1.246634 0.909941 0.207 Uiso 1 1 d G U . . .
H1WB H 1.452951 1.298424 0.882372 0.207 Uiso 1 1 d G U . . .
O2W O 1.0561(2) 1.2482(3) 1.05830(17) 0.0265(8) Uani 1 1 d . . . . .
H2WA H 1.004433 1.255752 1.058710 0.040 Uiso 1 1 d R U . . .
H2WB H 1.069242 1.214840 1.085800 0.040 Uiso 1 1 d R U . . .
C1 C 0.7492(3) 0.9504(3) 1.0403(2) 0.0224(11) Uani 1 1 d . . . . .
H1A H 0.724057 0.938321 1.079350 0.027 Uiso 1 1 calc R U . . .
H1B H 0.717783 0.976072 1.018292 0.027 Uiso 1 1 calc R U . . .
C2 C 0.6346(3) 0.7836(3) 1.0235(3) 0.0231(11) Uani 1 1 d . . . . .
H2 H 0.627985 0.768420 1.064944 0.028 Uiso 1 1 calc R U . . .
C3 C 0.6300(4) 0.7037(3) 0.9912(3) 0.0306(13) Uani 1 1 d . . . . .
H3A H 0.680656 0.695319 1.002885 0.046 Uiso 1 1 calc R U . . .
H3B H 0.633885 0.715796 0.950328 0.046 Uiso 1 1 calc R U . . .
H3C H 0.572483 0.648498 0.999797 0.046 Uiso 1 1 calc R U . . .
C4 C 0.5615(3) 0.8065(3) 1.0075(3) 0.0249(12) Uani 1 1 d . . . . .
H4 H 0.571838 0.859743 1.031119 0.030 Uiso 1 1 calc R U . . .
C5 C 0.5604(4) 0.8316(4) 0.9459(3) 0.0344(14) Uani 1 1 d . . . . .
H5A H 0.553622 0.781418 0.921223 0.041 Uiso 1 1 calc R U . . .
H5B H 0.618884 0.886335 0.936472 0.041 Uiso 1 1 calc R U . . .
C6 C 0.4818(5) 0.8502(6) 0.9342(4) 0.0493(19) Uani 1 1 d . . . . .
H6A H 0.492732 0.904819 0.955648 0.059 Uiso 1 1 calc R U . . .
H6B H 0.481102 0.863053 0.893233 0.059 Uiso 1 1 calc R U . . .
C7 C 0.3911(5) 0.7721(6) 0.9507(4) 0.057(2) Uani 1 1 d . . . . .
H7A H 0.376705 0.718769 0.926676 0.068 Uiso 1 1 calc R U . . .
H7B H 0.343491 0.788442 0.944643 0.068 Uiso 1 1 calc R U . . .
C8 C 0.3929(4) 0.7485(5) 1.0134(4) 0.052(2) Uani 1 1 d . . . . .
H8A H 0.402782 0.800377 1.037492 0.062 Uiso 1 1 calc R U . . .
H8B H 0.333716 0.695519 1.023910 0.062 Uiso 1 1 calc R U . . .
C9 C 0.4684(4) 0.7267(4) 1.0239(3) 0.0395(16) Uani 1 1 d . . . . .
H9A H 0.456385 0.672649 1.001455 0.047 Uiso 1 1 calc R U . . .
H9B H 0.468915 0.712227 1.064630 0.047 Uiso 1 1 calc R U . . .
C10 C 1.1772(3) 1.2467(3) 0.9291(2) 0.0189(10) Uani 1 1 d . U . . .
H10A H 1.225642 1.297903 0.950762 0.023 Uiso 1 1 calc R U . . .
H10B H 1.194022 1.256307 0.888350 0.023 Uiso 1 1 calc R U . . .
C11 C 1.0936(4) 1.3330(3) 0.9191(2) 0.0209(10) Uani 1 1 d . U . . .
H11 H 1.125899 1.351712 0.881821 0.025 Uiso 1 1 calc R U . . .
C12 C 1.1475(4) 1.4067(4) 0.9615(3) 0.0294(13) Uani 1 1 d . . . . .
H12A H 1.117294 1.389866 0.998563 0.044 Uiso 1 1 calc R U . . .
H12B H 1.151963 1.463599 0.948649 0.044 Uiso 1 1 calc R U . . .
H12C H 1.208580 1.414841 0.964878 0.044 Uiso 1 1 calc R U . . .
C13 C 0.9962(4) 1.3146(3) 0.9100(2) 0.0228(11) Uani 1 1 d . . . . .
H13 H 0.966505 1.263502 0.882269 0.027 Uiso 1 1 calc R U . . .
C14 C 0.9982(4) 1.3968(4) 0.8827(3) 0.0343(14) Uani 1 1 d . . . . .
H14A H 1.028833 1.449376 0.908704 0.041 Uiso 1 1 calc R U . . .
H14B H 1.034025 1.412194 0.847137 0.041 Uiso 1 1 calc R U . . .
C15 C 0.9041(5) 1.3798(4) 0.8694(3) 0.0437(18) Uani 1 1 d . . . . .
H15A H 0.908459 1.436315 0.854642 0.052 Uiso 1 1 calc R U . . .
H15B H 0.876692 1.332962 0.839387 0.052 Uiso 1 1 calc R U . . .
C16 C 0.8437(5) 1.3489(5) 0.9208(3) 0.0426(17) Uani 1 1 d . . . . .
H16A H 0.781334 1.332744 0.909500 0.051 Uiso 1 1 calc R U . . .
H16B H 0.865774 1.399268 0.948584 0.051 Uiso 1 1 calc R U . . .
C17 C 0.8416(4) 1.2668(4) 0.9490(3) 0.0338(14) Uani 1 1 d . . . . .
H17A H 0.805000 1.251235 0.984187 0.041 Uiso 1 1 calc R U . . .
H17B H 0.812128 1.214059 0.922987 0.041 Uiso 1 1 calc R U . . .
C18 C 0.9371(4) 1.2858(4) 0.9633(3) 0.0273(12) Uani 1 1 d . . . . .
H18A H 0.964579 1.334495 0.992233 0.033 Uiso 1 1 calc R U . . .
H18B H 0.933851 1.230478 0.979470 0.033 Uiso 1 1 calc R U . . .
C19 C 1.2211(4) 0.9179(4) 0.9090(3) 0.0298(14) Uani 1 1 d . . . . .
H19A H 1.246618 0.916785 0.946620 0.036 Uiso 1 1 calc R U . . .
H19B H 1.231359 0.877587 0.883525 0.036 Uiso 1 1 calc R U . . .
C20 C 1.3720(4) 1.0433(4) 0.8739(3) 0.0286(12) Uani 1 1 d . . . . .
H20 H 1.398193 1.102760 0.853579 0.034 Uiso 1 1 calc R U . . .
C21 C 1.3774(4) 0.9755(4) 0.8343(4) 0.0426(16) Uani 1 1 d . . . . .
H21A H 1.329818 0.955796 0.805319 0.064 Uiso 1 1 calc R U . . .
H21B H 1.368918 0.922872 0.856179 0.064 Uiso 1 1 calc R U . . .
H21C H 1.436982 1.004307 0.815753 0.064 Uiso 1 1 calc R U . . .
C22 C 1.4302(4) 1.0571(5) 0.9276(3) 0.0468(18) Uani 1 1 d . . . . .
H22 H 1.405565 0.997375 0.947376 0.056 Uiso 1 1 calc R U . . .
C23 C 1.5280(5) 1.0893(7) 0.9107(5) 0.074(3) Uani 1 1 d . U . . .
H23A H 1.552494 1.147332 0.889719 0.089 Uiso 1 1 calc R U . . .
H23B H 1.529430 1.044116 0.884855 0.089 Uiso 1 1 calc R U . . .
C24 C 1.5895(6) 1.1031(7) 0.9632(5) 0.086(3) Uani 1 1 d . U . . .
H24A H 1.570178 1.044155 0.981952 0.104 Uiso 1 1 calc R U . . .
H24B H 1.653451 1.129020 0.950967 0.104 Uiso 1 1 calc R U . . .
C25 C 1.5814(6) 1.1656(7) 1.0032(5) 0.089(3) Uani 1 1 d . U . . .
H25A H 1.621109 1.175513 1.036383 0.107 Uiso 1 1 calc R U . . .
H25B H 1.603384 1.224963 0.984253 0.107 Uiso 1 1 calc R U . . .
C26 C 1.4879(6) 1.1320(8) 1.0234(5) 0.091(3) Uani 1 1 d . U . . .
H26A H 1.485628 1.175991 1.049912 0.109 Uiso 1 1 calc R U . . .
H26B H 1.464550 1.073108 1.043096 0.109 Uiso 1 1 calc R U . . .
C27 C 1.4284(6) 1.1205(7) 0.9665(4) 0.072(3) Uani 1 1 d . U . . .
H27A H 1.364849 1.099678 0.977523 0.086 Uiso 1 1 calc R U . . .
H27B H 1.452832 1.180163 0.947549 0.086 Uiso 1 1 calc R U . . .
C28 C 1.1705(4) 0.6873(4) 0.8516(3) 0.0392(15) Uani 1 1 d . . . . .
C29 C 1.2099(5) 0.6267(5) 0.8411(4) 0.056(2) Uani 1 1 d . . . . .
H29A H 1.267541 0.660682 0.820618 0.084 Uiso 1 1 calc R U . . .
H29B H 1.167416 0.574318 0.818288 0.084 Uiso 1 1 calc R U . . .
H29C H 1.220512 0.605615 0.877522 0.084 Uiso 1 1 calc R U . . .
N1 N 0.7298(3) 0.8632(3) 1.01398(19) 0.0185(9) Uani 1 1 d . . . . .
H1C H 0.770372 0.847908 1.027785 0.022 Uiso 1 1 calc R U . . .
H1D H 0.739406 0.871987 0.975886 0.022 Uiso 1 1 calc R U . . .
N2 N 1.0898(3) 1.2454(3) 0.93728(19) 0.0179(8) Uani 1 1 d . U . . .
H2A H 1.074008 1.235173 0.974640 0.021 Uiso 1 1 calc R U . . .
H2B H 1.045701 1.198599 0.916972 0.021 Uiso 1 1 calc R U . . .
N3 N 1.2728(3) 1.0112(3) 0.8865(2) 0.0220(9) Uani 1 1 d . . . . .
H3D H 1.269946 1.049812 0.912052 0.026 Uiso 1 1 calc R U . . .
H3E H 1.245693 1.014441 0.853890 0.026 Uiso 1 1 calc R U . . .
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'
N N 0.0061 0.0033 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 '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
O7 Tb1 O5 80.43(13) . 5_565 ?
O7 Tb1 O8 86.00(13) . 5_565 ?
O5 Tb1 O8 81.07(13) 5_565 5_565 ?
O7 Tb1 O1 84.05(13) . 6_654 ?
O5 Tb1 O1 156.80(10) 5_565 6_654 ?
O8 Tb1 O1 80.73(13) 5_565 6_654 ?
O7 Tb1 O2 155.25(13) . . ?
O5 Tb1 O2 123.07(13) 5_565 . ?
O8 Tb1 O2 104.04(12) 5_565 . ?
O1 Tb1 O2 75.54(11) 6_654 . ?
O7 Tb1 O4 93.86(13) . . ?
O5 Tb1 O4 71.84(11) 5_565 . ?
O8 Tb1 O4 152.51(12) 5_565 . ?
O1 Tb1 O4 126.65(13) 6_654 . ?
O2 Tb1 O4 87.38(11) . . ?
O7 Tb1 O5 73.90(13) . . ?
O5 Tb1 O5 121.17(13) 5_565 . ?
O8 Tb1 O5 145.70(13) 5_565 . ?
O1 Tb1 O5 69.95(12) 6_654 . ?
O2 Tb1 O5 85.89(11) . . ?
O4 Tb1 O5 58.53(12) . . ?
O7 Tb1 O1 145.20(13) . . ?
O5 Tb1 O1 69.56(12) 5_565 . ?
O8 Tb1 O1 72.61(12) 5_565 . ?
O1 Tb1 O1 117.87(12) 6_654 . ?
O2 Tb1 O1 59.13(12) . . ?
O4 Tb1 O1 93.16(11) . . ?
O5 Tb1 O1 137.04(10) . . ?
O7 Tb1 Tb1 72.70(10) . 6_654 ?
O5 Tb1 Tb1 147.24(10) 5_565 6_654 ?
O8 Tb1 Tb1 114.64(9) 5_565 6_654 ?
O1 Tb1 Tb1 37.22(10) 6_654 6_654 ?
O2 Tb1 Tb1 82.56(8) . 6_654 ?
O4 Tb1 Tb1 91.33(8) . 6_654 ?
O5 Tb1 Tb1 33.05(9) . 6_654 ?
O1 Tb1 Tb1 141.12(8) . 6_654 ?
O7 Tb1 Tb1 112.86(10) . 5_565 ?
O5 Tb1 Tb1 35.56(10) 5_565 5_565 ?
O8 Tb1 Tb1 70.33(9) 5_565 5_565 ?
O1 Tb1 Tb1 144.64(9) 6_654 5_565 ?
O2 Tb1 Tb1 91.88(8) . 5_565 ?
O4 Tb1 Tb1 84.59(8) . 5_565 ?
O5 Tb1 Tb1 143.11(9) . 5_565 ?
O1 Tb1 Tb1 34.31(9) . 5_565 ?
Tb1 Tb1 Tb1 173.266(2) 6_654 5_565 ?
O3 P1 O2 115.5(2) . . ?
O3 P1 O1 115.5(2) . . ?
O2 P1 O1 105.9(2) . . ?
O3 P1 C1 104.4(2) . . ?
O2 P1 C1 109.6(2) . . ?
O1 P1 C1 105.4(2) . . ?
O6 P2 O5 115.5(2) . . ?
O6 P2 O4 116.3(2) . . ?
O5 P2 O4 104.4(2) . . ?
O6 P2 C10 106.5(2) . . ?
O5 P2 C10 106.7(2) . . ?
O4 P2 C10 106.9(2) . . ?
O9 P3 O8 112.8(2) . . ?
O9 P3 O7 109.9(2) . . ?
O8 P3 O7 114.68(18) . . ?
O9 P3 C19 104.8(2) . . ?
O8 P3 C19 106.6(3) . . ?
O7 P3 C19 107.3(3) . . ?
P1 O1 Tb1 151.7(2) . 5_565 ?
P1 O1 Tb1 95.10(18) . . ?
Tb1 O1 Tb1 108.46(14) 5_565 . ?
P1 O2 Tb1 99.57(17) . . ?
P2 O4 Tb1 97.77(16) . . ?
P2 O5 Tb1 150.8(2) . 6_654 ?
P2 O5 Tb1 97.77(19) . . ?
Tb1 O5 Tb1 111.39(15) 6_654 . ?
P3 O7 Tb1 137.4(2) . . ?
P3 O8 Tb1 138.3(2) . 6_654 ?
C28 O10 H10C 110.5 . . ?
H1WA O1W H1WB 104.1 . . ?
H2WA O2W H2WB 125.5 . . ?
N1 C1 P1 113.5(3) . . ?
N1 C1 H1A 108.9 . . ?
P1 C1 H1A 108.9 . . ?
N1 C1 H1B 108.9 . . ?
P1 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
N1 C2 C4 112.2(4) . . ?
N1 C2 C3 106.1(4) . . ?
C4 C2 C3 114.9(5) . . ?
N1 C2 H2 107.8 . . ?
C4 C2 H2 107.8 . . ?
C3 C2 H2 107.8 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C5 C4 C2 115.8(5) . . ?
C5 C4 C9 109.7(5) . . ?
C2 C4 C9 109.0(4) . . ?
C5 C4 H4 107.3 . . ?
C2 C4 H4 107.3 . . ?
C9 C4 H4 107.3 . . ?
C4 C5 C6 111.2(5) . . ?
C4 C5 H5A 109.4 . . ?
C6 C5 H5A 109.4 . . ?
C4 C5 H5B 109.4 . . ?
C6 C5 H5B 109.4 . . ?
H5A C5 H5B 108.0 . . ?
C7 C6 C5 112.6(6) . . ?
C7 C6 H6A 109.1 . . ?
C5 C6 H6A 109.1 . . ?
C7 C6 H6B 109.1 . . ?
C5 C6 H6B 109.1 . . ?
H6A C6 H6B 107.8 . . ?
C6 C7 C8 109.6(6) . . ?
C6 C7 H7A 109.8 . . ?
C8 C7 H7A 109.8 . . ?
C6 C7 H7B 109.8 . . ?
C8 C7 H7B 109.8 . . ?
H7A C7 H7B 108.2 . . ?
C9 C8 C7 110.4(6) . . ?
C9 C8 H8A 109.6 . . ?
C7 C8 H8A 109.6 . . ?
C9 C8 H8B 109.6 . . ?
C7 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
C8 C9 C4 111.5(5) . . ?
C8 C9 H9A 109.3 . . ?
C4 C9 H9A 109.3 . . ?
C8 C9 H9B 109.3 . . ?
C4 C9 H9B 109.3 . . ?
H9A C9 H9B 108.0 . . ?
N2 C10 P2 111.2(3) . . ?
N2 C10 H10A 109.4 . . ?
P2 C10 H10A 109.4 . . ?
N2 C10 H10B 109.4 . . ?
P2 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
C12 C11 N2 110.0(4) . . ?
C12 C11 C13 114.0(4) . . ?
N2 C11 C13 109.0(4) . . ?
C12 C11 H11 107.9 . . ?
N2 C11 H11 107.9 . . ?
C13 C11 H11 107.9 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C18 110.6(4) . . ?
C14 C13 C11 110.2(4) . . ?
C18 C13 C11 114.8(5) . . ?
C14 C13 H13 107.0 . . ?
C18 C13 H13 107.0 . . ?
C11 C13 H13 107.0 . . ?
C15 C14 C13 112.1(5) . . ?
C15 C14 H14A 109.2 . . ?
C13 C14 H14A 109.2 . . ?
C15 C14 H14B 109.2 . . ?
C13 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
C16 C15 C14 112.0(6) . . ?
C16 C15 H15A 109.2 . . ?
C14 C15 H15A 109.2 . . ?
C16 C15 H15B 109.2 . . ?
C14 C15 H15B 109.2 . . ?
H15A C15 H15B 107.9 . . ?
C15 C16 C17 111.5(5) . . ?
C15 C16 H16A 109.3 . . ?
C17 C16 H16A 109.3 . . ?
C15 C16 H16B 109.3 . . ?
C17 C16 H16B 109.3 . . ?
H16A C16 H16B 108.0 . . ?
C18 C17 C16 111.5(5) . . ?
C18 C17 H17A 109.3 . . ?
C16 C17 H17A 109.3 . . ?
C18 C17 H17B 109.3 . . ?
C16 C17 H17B 109.3 . . ?
H17A C17 H17B 108.0 . . ?
C13 C18 C17 110.2(5) . . ?
C13 C18 H18A 109.6 . . ?
C17 C18 H18A 109.6 . . ?
C13 C18 H18B 109.6 . . ?
C17 C18 H18B 109.6 . . ?
H18A C18 H18B 108.1 . . ?
N3 C19 P3 116.8(3) . . ?
N3 C19 H19A 108.1 . . ?
P3 C19 H19A 108.1 . . ?
N3 C19 H19B 108.1 . . ?
P3 C19 H19B 108.1 . . ?
H19A C19 H19B 107.3 . . ?
C21 C20 N3 108.9(4) . . ?
C21 C20 C22 109.9(5) . . ?
N3 C20 C22 114.0(5) . . ?
C21 C20 H20 108.0 . . ?
N3 C20 H20 108.0 . . ?
C22 C20 H20 108.0 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C27 C22 C23 109.2(7) . . ?
C27 C22 C20 112.7(6) . . ?
C23 C22 C20 110.0(7) . . ?
C27 C22 H22 108.3 . . ?
C23 C22 H22 108.3 . . ?
C20 C22 H22 108.3 . . ?
C22 C23 C24 112.2(8) . . ?
C22 C23 H23A 109.2 . . ?
C24 C23 H23A 109.2 . . ?
C22 C23 H23B 109.2 . . ?
C24 C23 H23B 109.2 . . ?
H23A C23 H23B 107.9 . . ?
C25 C24 C23 108.4(8) . . ?
C25 C24 H24A 110.0 . . ?
C23 C24 H24A 110.0 . . ?
C25 C24 H24B 110.0 . . ?
C23 C24 H24B 110.0 . . ?
H24A C24 H24B 108.4 . . ?
C26 C25 C24 113.4(8) . . ?
C26 C25 H25A 108.9 . . ?
C24 C25 H25A 108.9 . . ?
C26 C25 H25B 108.9 . . ?
C24 C25 H25B 108.9 . . ?
H25A C25 H25B 107.7 . . ?
C25 C26 C27 105.5(9) . . ?
C25 C26 H26A 110.6 . . ?
C27 C26 H26A 110.6 . . ?
C25 C26 H26B 110.6 . . ?
C27 C26 H26B 110.6 . . ?
H26A C26 H26B 108.8 . . ?
C22 C27 C26 111.8(7) . . ?
C22 C27 H27A 109.3 . . ?
C26 C27 H27A 109.3 . . ?
C22 C27 H27B 109.3 . . ?
C26 C27 H27B 109.3 . . ?
H27A C27 H27B 107.9 . . ?
O11 C28 O10 123.4(6) . . ?
O11 C28 C29 123.7(7) . . ?
O10 C28 C29 112.9(6) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C1 N1 C2 115.7(4) . . ?
C1 N1 H1C 108.4 . . ?
C2 N1 H1C 108.4 . . ?
C1 N1 H1D 108.4 . . ?
C2 N1 H1D 108.4 . . ?
H1C N1 H1D 107.4 . . ?
C10 N2 C11 113.4(4) . . ?
C10 N2 H2A 108.9 . . ?
C11 N2 H2A 108.9 . . ?
C10 N2 H2B 108.9 . . ?
C11 N2 H2B 108.9 . . ?
H2A N2 H2B 107.7 . . ?
C19 N3 C20 114.4(4) . . ?
C19 N3 H3D 108.7 . . ?
C20 N3 H3D 108.7 . . ?
C19 N3 H3E 108.7 . . ?
C20 N3 H3E 108.7 . . ?
H3D N3 H3E 107.6 . . ?
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
Tb1 O7 2.271(4) . ?
Tb1 O5 2.313(4) 5_565 ?
Tb1 O8 2.328(4) 5_565 ?
Tb1 O1 2.347(4) 6_654 ?
Tb1 O2 2.413(3) . ?
Tb1 O4 2.465(3) . ?
Tb1 O5 2.466(4) . ?
Tb1 O1 2.518(4) . ?
Tb1 Tb1 3.94884(18) 6_654 ?
Tb1 Tb1 3.94892(15) 5_565 ?
P1 O3 1.505(4) . ?
P1 O2 1.522(4) . ?
P1 O1 1.528(4) . ?
P1 C1 1.827(5) . ?
P2 O6 1.497(4) . ?
P2 O5 1.525(4) . ?
P2 O4 1.527(4) . ?
P2 C10 1.827(5) . ?
P3 O9 1.512(4) . ?
P3 O8 1.519(4) . ?
P3 O7 1.520(4) . ?
P3 C19 1.827(6) . ?
O10 C28 1.291(8) . ?
O10 H10C 0.8829 . ?
O11 C28 1.197(8) . ?
O1W H1WA 0.9492 . ?
O1W H1WB 0.9493 . ?
O2W H2WA 0.9495 . ?
O2W H2WB 0.9579 . ?
C1 N1 1.485(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N1 1.522(6) . ?
C2 C4 1.525(7) . ?
C2 C3 1.525(7) . ?
C2 H2 1.0000 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C5 1.514(8) . ?
C4 C9 1.533(7) . ?
C4 H4 1.0000 . ?
C5 C6 1.545(8) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.499(11) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.533(11) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.526(8) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 N2 1.490(6) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.503(8) . ?
C11 N2 1.519(6) . ?
C11 C13 1.540(7) . ?
C11 H11 1.0000 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.523(7) . ?
C13 C18 1.527(8) . ?
C13 H13 1.0000 . ?
C14 C15 1.511(8) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.502(10) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.529(8) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.529(8) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 N3 1.477(7) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.521(9) . ?
C20 N3 1.521(7) . ?
C20 C22 1.549(9) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C27 1.426(12) . ?
C22 C23 1.522(10) . ?
C22 H22 1.0000 . ?
C23 C24 1.559(13) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.477(13) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.475(13) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.629(12) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.505(9) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
N1 H1C 0.9100 . ?
N1 H1D 0.9100 . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N3 H3D 0.9100 . ?
N3 H3E 0.9100 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O10 H10C O9 0.88 1.64 2.511(6) 167.3 . yes
O1W H1WA O6 0.95 1.86 2.775(9) 160.3 . yes
O2W H2WA O3 0.95 2.31 2.786(5) 110.4 . yes
O2W H2WB O2 0.96 1.96 2.869(5) 156.7 5_565 yes
N1 H1D O3 0.91 1.75 2.657(6) 171.8 6_654 yes
N1 H1C O8 0.91 2.28 3.147(5) 158.9 5_565 yes
N2 H2A O2W 0.91 2.02 2.910(6) 165.0 . yes
N2 H2B O4 0.91 1.92 2.732(6) 148.4 6_654 yes
N3 H3D O6 0.91 1.96 2.838(6) 161.6 . yes
N3 H3E O9 0.91 2.40 3.120(6) 136.1 6_654 yes
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
O3 P1 O1 Tb1 12.7(5) . . . 5_565 ?
O2 P1 O1 Tb1 141.9(4) . . . 5_565 ?
C1 P1 O1 Tb1 -102.0(5) . . . 5_565 ?
O3 P1 O1 Tb1 -134.05(18) . . . . ?
O2 P1 O1 Tb1 -4.79(19) . . . . ?
C1 P1 O1 Tb1 111.3(2) . . . . ?
O3 P1 O2 Tb1 134.31(18) . . . . ?
O1 P1 O2 Tb1 5.0(2) . . . . ?
C1 P1 O2 Tb1 -108.1(2) . . . . ?
O6 P2 O4 Tb1 -117.21(19) . . . . ?
O5 P2 O4 Tb1 11.29(19) . . . . ?
C10 P2 O4 Tb1 124.05(18) . . . . ?
O6 P2 O5 Tb1 -62.2(5) . . . 6_654 ?
O4 P2 O5 Tb1 168.8(4) . . . 6_654 ?
C10 P2 O5 Tb1 55.9(4) . . . 6_654 ?
O6 P2 O5 Tb1 117.7(2) . . . . ?
O4 P2 O5 Tb1 -11.28(18) . . . . ?
C10 P2 O5 Tb1 -124.18(19) . . . . ?
O9 P3 O7 Tb1 -112.7(3) . . . . ?
O8 P3 O7 Tb1 15.6(5) . . . . ?
C19 P3 O7 Tb1 133.8(3) . . . . ?
O9 P3 O8 Tb1 145.7(3) . . . 6_654 ?
O7 P3 O8 Tb1 18.8(4) . . . 6_654 ?
C19 P3 O8 Tb1 -99.8(4) . . . 6_654 ?
O3 P1 C1 N1 177.5(4) . . . . ?
O2 P1 C1 N1 53.2(4) . . . . ?
O1 P1 C1 N1 -60.3(4) . . . . ?
N1 C2 C4 C5 61.4(6) . . . . ?
C3 C2 C4 C5 -59.8(6) . . . . ?
N1 C2 C4 C9 -174.3(5) . . . . ?
C3 C2 C4 C9 64.4(7) . . . . ?
C2 C4 C5 C6 178.1(5) . . . . ?
C9 C4 C5 C6 54.3(7) . . . . ?
C4 C5 C6 C7 -55.7(9) . . . . ?
C5 C6 C7 C8 56.0(9) . . . . ?
C6 C7 C8 C9 -57.2(8) . . . . ?
C7 C8 C9 C4 58.5(8) . . . . ?
C5 C4 C9 C8 -56.9(7) . . . . ?
C2 C4 C9 C8 175.4(6) . . . . ?
O6 P2 C10 N2 -177.8(4) . . . . ?
O5 P2 C10 N2 58.3(4) . . . . ?
O4 P2 C10 N2 -52.9(4) . . . . ?
C12 C11 C13 C14 65.9(7) . . . . ?
N2 C11 C13 C14 -170.8(5) . . . . ?
C12 C11 C13 C18 -59.7(6) . . . . ?
N2 C11 C13 C18 63.6(6) . . . . ?
C18 C13 C14 C15 -55.7(7) . . . . ?
C11 C13 C14 C15 176.3(5) . . . . ?
C13 C14 C15 C16 54.4(7) . . . . ?
C14 C15 C16 C17 -53.4(8) . . . . ?
C15 C16 C17 C18 54.8(8) . . . . ?
C14 C13 C18 C17 56.3(6) . . . . ?
C11 C13 C18 C17 -178.3(4) . . . . ?
C16 C17 C18 C13 -56.1(7) . . . . ?
O9 P3 C19 N3 164.5(4) . . . . ?
O8 P3 C19 N3 44.7(5) . . . . ?
O7 P3 C19 N3 -78.6(5) . . . . ?
C21 C20 C22 C27 179.7(7) . . . . ?
N3 C20 C22 C27 -57.8(8) . . . . ?
C21 C20 C22 C23 57.6(8) . . . . ?
N3 C20 C22 C23 -179.9(6) . . . . ?
C27 C22 C23 C24 56.7(10) . . . . ?
C20 C22 C23 C24 -179.2(7) . . . . ?
C22 C23 C24 C25 -54.8(11) . . . . ?
C23 C24 C25 C26 59.5(13) . . . . ?
C24 C25 C26 C27 -60.2(13) . . . . ?
C23 C22 C27 C26 -59.0(11) . . . . ?
C20 C22 C27 C26 178.5(7) . . . . ?
C25 C26 C27 C22 60.6(12) . . . . ?
P1 C1 N1 C2 164.9(4) . . . . ?
C4 C2 N1 C1 52.0(6) . . . . ?
C3 C2 N1 C1 178.2(5) . . . . ?
P2 C10 N2 C11 179.0(4) . . . . ?
C12 C11 N2 C10 -73.1(6) . . . . ?
C13 C11 N2 C10 161.1(4) . . . . ?
P3 C19 N3 C20 -173.0(4) . . . . ?
C21 C20 N3 C19 54.6(7) . . . . ?
C22 C20 N3 C19 -68.4(7) . . . . ?
