#------------------------------------------------------------------------------
#$Date: 2019-11-07 23:04:00 +0100 (jue 07 de nov de 2019) $
#$Revision: 224177 $
#$URL: svn://www.crystallography.net/cod/cif/7/04/95/7049547.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_7049547
loop_
_publ_author_name
'Biswas, Sourav'
'Kumar, Pawan'
'Swain, Abinash'
'Gupta, Tulika'
'Kalita, Pankaj'
'Kundu, Subrata'
'Rajaraman, Gopalan'
'Chandrasekhar, Vadapalli'
_publ_section_title
;
 Phosphonate-assisted tetranuclear lanthanide assemblies: observation of
 the toroidic ground state in the TbIII analogue.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6421
_journal_page_last               6434
_journal_paper_doi               10.1039/c9dt00592g
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'C55.62 H69.24 F6 N10 O20 P2 Tb4, 2(Cl), 0.38(H2 O)'
_chemical_formula_sum            'C55.62 H70 Cl2 F6 N10 O20.38 P2 Tb4'
_chemical_formula_weight         2087.25
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-29 deposited with the CCDC.    2019-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                112.5610(10)
_cell_angle_beta                 99.3550(10)
_cell_angle_gamma                108.9880(10)
_cell_formula_units_Z            1
_cell_length_a                   12.2855(5)
_cell_length_b                   12.8600(5)
_cell_length_c                   14.6338(6)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.37
_cell_measurement_theta_min      2.79
_cell_volume                     1906.44(14)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29176
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.378
_diffrn_reflns_theta_min         2.734
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.862
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6034
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0681 before and 0.0450 after correction.
The Ratio of minimum to maximum transmission is 0.8092.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.818
_exptl_crystal_description       block
_exptl_crystal_F_000             1015
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.011
_refine_diff_density_max         1.294
_refine_diff_density_min         -1.136
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         9554
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0337P)²+2.4541P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0747
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7817
_reflns_number_total             9554
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt00592g2.cif
_cod_data_source_block           complex2_sq
_cod_depositor_comments
'Adding full bibliography for 7049546--7049548.cif.'
_cod_original_cell_volume        1906.43(13)
_cod_database_code               7049547
_shelx_shelxl_version_number     2017/1
_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_max   0.959
_shelx_estimated_absorpt_t_min   0.614
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O17-H17
 0.87 with sigma of 0.01
 O3-H3
 0.87 with sigma of 0.01
 C26-H17
 1.916347 with sigma of 0.02
 Tb2-H17
 3.015924 with sigma of 0.02
 C1AA-H3
 1.917636 with sigma of 0.02
 Tb1-H3
 2.869836 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O3) = Uanis(O0AA)
4. Others
 Fixed Sof: O3(0.81) H3(0.81) C1AA(0.81) H1AA(0.81) H1AB(0.81) H1AC(0.81)
 O1AA(0.19) H1AD(0.19) H1AE(0.19) O0AA(0.19) H0AA(0.19) H0AB(0.19)
5.a Riding coordinates:
 O1AA(H1AD,H1AE)
5.b Rotating group:
 O0AA(H0AA,H0AB)
5.c Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C28(H28A,H28B), C29(H29A,H29B), C26(H26A,H26B), C27(H27A,H27B)
5.d Aromatic/amide H refined with riding coordinates:
 N2(H2), C7(H7), C5(H5), C15(H15), C10(H10), C14(H14), C13(H13), C6(H6),
 C24(H24), C23(H23)
5.e Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C20(H20A,H20B,H20C), C1AA(H1AA,H1AB,
 H1AC)
;
_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_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.55764(2) 1.01151(2) 0.32150(2) 0.01594(5) Uani 1 1 d D . . .
Tb2 Tb 0.25404(2) 0.79463(2) 0.35092(2) 0.01643(5) Uani 1 1 d D . . .
P1 P 0.56650(8) 0.88750(9) 0.47240(7) 0.01566(19) Uani 1 1 d . . . .
Cl1 Cl 0.26657(12) 0.61770(13) 0.01891(9) 0.0502(3) Uani 1 1 d . . . .
O4 O 0.4649(2) 0.8460(2) 0.37083(19) 0.0171(5) Uani 1 1 d . . . .
O2 O 0.7592(2) 1.0320(2) 0.3419(2) 0.0203(5) Uani 1 1 d . . . .
O5 O 0.3402(2) 0.9821(2) 0.50145(19) 0.0175(5) Uani 1 1 d . . . .
O6 O 0.2793(2) 0.6661(2) 0.4239(2) 0.0214(6) Uani 1 1 d . . . .
O3 O 0.5147(7) 0.8295(10) 0.1679(7) 0.0215(14) Uani 0.81 1 d D P A 1
H3 H 0.443(2) 0.767(2) 0.140(3) 0.032 Uiso 0.81 1 d DR P B 1
O1 O 0.4804(2) 1.1121(2) 0.43857(19) 0.0169(5) Uani 1 1 d . . . .
O9 O 0.3274(2) 0.8982(2) 0.2548(2) 0.0193(5) Uani 1 1 d . . . .
O15 O 0.3226(2) 0.7666(2) 0.5984(2) 0.0216(6) Uani 1 1 d . . . .
O11 O 0.1274(2) 0.8016(3) 0.4604(2) 0.0221(6) Uani 1 1 d . . . .
H11 H 0.157(4) 0.847(4) 0.520(4) 0.033 Uiso 1 1 d R . . .
N8 N 0.4336(3) 1.0487(3) 0.1892(2) 0.0175(6) Uani 1 1 d . . . .
F1 F 0.2960(3) 0.4739(2) 0.4443(2) 0.0537(8) Uani 1 1 d . . . .
N10 N 0.0922(3) 0.8027(3) 0.2217(2) 0.0200(7) Uani 1 1 d . . . .
C3 C 0.0368(4) 0.6959(4) 0.4584(3) 0.0280(9) Uani 1 1 d . . . .
H3A H -0.037505 0.709154 0.463025 0.034 Uiso 1 1 calc R . . .
H3B H 0.068124 0.684454 0.518966 0.034 Uiso 1 1 calc R . . .
N2 N 0.3088(3) 1.0120(3) 0.1682(2) 0.0194(7) Uani 1 1 d . . . .
H2 H 0.265531 1.038141 0.136065 0.023 Uiso 1 1 calc R . . .
N7 N 0.6575(3) 1.0852(3) 0.2040(2) 0.0186(6) Uani 1 1 d . . . .
C1 C 0.2966(3) 0.6765(4) 0.5145(3) 0.0197(8) Uani 1 1 d . . . .
C9 C 0.2647(3) 0.9328(3) 0.2031(3) 0.0172(7) Uani 1 1 d . . . .
C17 C 0.7744(3) 1.1033(3) 0.2157(3) 0.0184(7) Uani 1 1 d . . . .
C12 C 0.8425(3) 1.1528(3) 0.1604(3) 0.0197(8) Uani 1 1 d . . . .
C16 C 0.8271(3) 1.0708(4) 0.2897(3) 0.0203(8) Uani 1 1 d . . . .
C4 C 0.1303(3) 0.8742(3) 0.1756(3) 0.0185(7) Uani 1 1 d . . . .
C7 C -0.1130(3) 0.7403(4) 0.1221(3) 0.0242(8) Uani 1 1 d . . . .
H7 H -0.197598 0.691827 0.104059 0.029 Uiso 1 1 calc R . . .
C5 C 0.0511(3) 0.8837(4) 0.1045(3) 0.0211(8) Uani 1 1 d . . . .
H5 H 0.081331 0.936044 0.074416 0.025 Uiso 1 1 calc R . . .
C15 C 0.9454(3) 1.0860(4) 0.3034(3) 0.0243(8) Uani 1 1 d . . . .
H15 H 0.982604 1.064270 0.351050 0.029 Uiso 1 1 calc R . . .
C10 C 0.4783(3) 1.0950(4) 0.1329(3) 0.0203(8) Uani 1 1 d . . . .
H10 H 0.430975 1.112729 0.087777 0.024 Uiso 1 1 calc R . . .
C11 C 0.6050(3) 1.1191(4) 0.1411(3) 0.0198(8) Uani 1 1 d . . . .
C14 C 0.9643(3) 1.1665(4) 0.1785(3) 0.0229(8) Uani 1 1 d . . . .
H14 H 1.012101 1.198761 0.142535 0.027 Uiso 1 1 calc R . . .
C8 C -0.0279(3) 0.7363(4) 0.1935(3) 0.0209(8) Uani 1 1 d . . . .
C13 C 0.7818(3) 1.1846(4) 0.0923(3) 0.0225(8) Uani 1 1 d . . . .
H13 H 0.822403 1.216146 0.052286 0.027 Uiso 1 1 calc R . . .
C6 C -0.0724(3) 0.8166(4) 0.0774(3) 0.0257(9) Uani 1 1 d . . . .
H6 H -0.128683 0.822442 0.028956 0.031 Uiso 1 1 calc R . . .
O17 O 0.2299(3) 0.6121(3) 0.2080(2) 0.0323(7) Uani 1 1 d D . . .
H17 H 0.237(3) 0.6052(19) 0.1472(13) 0.048 Uiso 1 1 d DR . . .
N1 N 0.0267(3) 0.6156(3) 0.2742(2) 0.0225(7) Uani 1 1 d . . . .
C18 C 0.6394(3) 0.7821(4) 0.4464(3) 0.0217(8) Uani 1 1 d . . . .
F3 F 0.1580(3) 0.4967(3) 0.5105(3) 0.0678(10) Uani 1 1 d . . . .
F2 F 0.3393(4) 0.5717(3) 0.6093(2) 0.0688(11) Uani 1 1 d . . . .
C24 C 1.0129(4) 1.1335(4) 0.2475(3) 0.0267(9) Uani 1 1 d . . . .
H24 H 1.094577 1.142699 0.258438 0.032 Uiso 1 1 calc R . . .
C23 C 0.6649(3) 1.1702(4) 0.0836(3) 0.0223(8) Uani 1 1 d . . . .
H23 H 0.624518 1.194127 0.039625 0.027 Uiso 1 1 calc R . . .
C19 C 0.6791(4) 0.7660(5) 0.3503(4) 0.0373(11) Uani 1 1 d . . . .
H19A H 0.608043 0.734325 0.289344 0.056 Uiso 1 1 calc GR . . .
H19B H 0.715948 0.706785 0.336856 0.056 Uiso 1 1 calc GR . . .
H19C H 0.738971 0.846443 0.362797 0.056 Uiso 1 1 calc GR . . .
C28 C -0.0666(3) 0.6574(4) 0.2464(3) 0.0256(9) Uani 1 1 d . . . .
H28A H -0.080863 0.706024 0.310724 0.031 Uiso 1 1 calc R . . .
H28B H -0.144302 0.583882 0.199052 0.031 Uiso 1 1 calc R . . .
C22 C 0.2748(4) 0.5541(4) 0.5193(3) 0.0305(9) Uani 1 1 d . . . .
C21 C 0.5489(4) 0.6560(4) 0.4284(4) 0.0316(10) Uani 1 1 d . . . .
H21A H 0.529072 0.665288 0.492507 0.047 Uiso 1 1 calc GR . . .
H21B H 0.585348 0.596568 0.410208 0.047 Uiso 1 1 calc GR . . .
H21C H 0.474371 0.625335 0.371047 0.047 Uiso 1 1 calc GR . . .
C29 C 0.0068(4) 0.5810(4) 0.3564(3) 0.0273(9) Uani 1 1 d . . . .
H29A H 0.058942 0.539370 0.367590 0.033 Uiso 1 1 calc R . . .
H29B H -0.079338 0.521641 0.334209 0.033 Uiso 1 1 calc R . . .
C20 C 0.7500(4) 0.8348(4) 0.5424(4) 0.0368(11) Uani 1 1 d . . . .
H20A H 0.809333 0.914578 0.553276 0.055 Uiso 1 1 calc GR . . .
H20B H 0.787543 0.776312 0.531375 0.055 Uiso 1 1 calc GR . . .
H20C H 0.724164 0.847231 0.604248 0.055 Uiso 1 1 calc GR . . .
C26 C 0.1343(4) 0.4959(4) 0.1855(4) 0.0387(11) Uani 1 1 d D . . .
H26A H 0.154397 0.473347 0.241495 0.046 Uiso 1 1 calc R . . .
H26B H 0.125994 0.428978 0.118245 0.046 Uiso 1 1 calc R . . .
C27 C 0.0176(4) 0.5098(4) 0.1790(4) 0.0333(10) Uani 1 1 d . . . .
H27A H -0.006475 0.522164 0.117418 0.040 Uiso 1 1 calc R . . .
H27B H -0.047105 0.432029 0.168451 0.040 Uiso 1 1 calc R . . .
C1AA C 0.5902(4) 0.7879(5) 0.1106(4) 0.0268(11) Uani 0.81 1 d D P A 1
H1AA H 0.593462 0.816423 0.057484 0.040 Uiso 0.81 1 calc GR P A 1
H1AB H 0.555651 0.696804 0.076354 0.040 Uiso 0.81 1 calc GR P A 1
H1AC H 0.672688 0.822216 0.159090 0.040 Uiso 0.81 1 calc GR P A 1
O1AA O 0.602(2) 0.746(2) 0.0127(19) 0.081(7) Uani 0.19 1 d . P C 2
H1AD H 0.570444 0.730123 -0.051497 0.121 Uiso 0.19 1 d R P C 2
H1AE H 0.603984 0.676993 0.007193 0.121 Uiso 0.19 1 d R P C 2
O0AA O 0.492(4) 0.817(5) 0.150(4) 0.0215(14) Uani 0.19 1 d . P A 2
H0AA H 0.553217 0.814509 0.125393 0.032 Uiso 0.19 1 d GR P A 2
H0AB H 0.437888 0.814150 0.099642 0.032 Uiso 0.19 1 d GR P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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
O4 Tb1 O5 57.05(8) . 2_676
O4 Tb1 O9 62.87(8) . .
O4 Tb1 N8 122.79(9) . .
O4 Tb1 N7 151.14(9) . .
O4 Tb1 O0AA 78.7(13) . .
O2 Tb1 O4 103.95(8) . .
O2 Tb1 O5 67.85(8) . 2_676
O2 Tb1 O3 82.1(2) . .
O2 Tb1 O9 156.28(9) . .
O2 Tb1 O15 76.48(9) . 2_676
O2 Tb1 N8 125.36(9) . .
O2 Tb1 N7 64.44(9) . .
O2 Tb1 O0AA 87.5(11) . .
O3 Tb1 O4 78.4(3) . .
O3 Tb1 O5 114.8(2) . 2_676
O3 Tb1 O9 76.0(2) . .
O3 Tb1 O15 139.4(3) . 2_676
O3 Tb1 N8 81.4(2) . .
O3 Tb1 N7 74.0(3) . .
O1 Tb1 O4 81.29(8) . .
O1 Tb1 O2 129.82(9) . .
O1 Tb1 O5 74.92(8) . 2_676
O1 Tb1 O3 145.7(2) . .
O1 Tb1 O9 70.18(9) . .
O1 Tb1 O15 69.91(9) . 2_676
O1 Tb1 N8 86.93(9) . .
O1 Tb1 N7 126.95(9) . .
O1 Tb1 O0AA 141.1(12) . .
O9 Tb1 O5 113.39(8) . 2_676
O9 Tb1 N8 60.46(9) . .
O9 Tb1 N7 116.82(9) . .
O9 Tb1 O0AA 71.1(11) . .
O15 Tb1 O4 140.11(8) 2_676 .
O15 Tb1 O5 88.38(8) 2_676 2_676
O15 Tb1 O9 126.65(9) 2_676 .
O15 Tb1 N8 83.51(9) 2_676 .
O15 Tb1 N7 65.73(9) 2_676 .
O15 Tb1 O0AA 140.3(13) 2_676 .
N8 Tb1 O5 161.74(9) . 2_676
N8 Tb1 N7 60.97(9) . .
N7 Tb1 O5 129.55(9) . 2_676
O0AA Tb1 N8 76.7(12) . .
O0AA Tb1 N7 74.6(13) . .
O4 Tb2 O11 137.77(9) . .
O4 Tb2 N10 129.79(9) . .
O4 Tb2 N1 147.33(9) . .
O5 Tb2 O4 80.47(8) . .
O5 Tb2 O6 99.16(9) . .
O5 Tb2 O9 90.07(9) . .
O5 Tb2 O11 68.68(9) . .
O5 Tb2 N10 107.70(9) . .
O5 Tb2 O17 162.02(10) . .
O5 Tb2 N1 128.29(9) . .
O6 Tb2 O4 81.85(8) . .
O6 Tb2 O9 145.30(9) . .
O6 Tb2 O11 75.64(9) . .
O6 Tb2 N10 140.78(9) . .
O6 Tb2 O17 75.13(10) . .
O6 Tb2 N1 78.63(9) . .
O9 Tb2 O4 66.70(8) . .
O9 Tb2 O11 138.13(9) . .
O9 Tb2 N10 63.91(9) . .
O9 Tb2 N1 120.88(9) . .
O11 Tb2 N10 87.94(9) . .
O11 Tb2 N1 60.69(10) . .
N10 Tb2 N1 62.36(10) . .
O17 Tb2 O4 81.83(9) . .
O17 Tb2 O9 85.83(10) . .
O17 Tb2 O11 124.56(10) . .
O17 Tb2 N10 86.17(11) . .
O17 Tb2 N1 68.00(10) . .
O4 P1 C18 109.43(16) . .
O5 P1 O4 105.13(14) 2_676 .
O5 P1 C18 109.10(16) 2_676 .
O1 P1 O4 113.26(14) 2_676 .
O1 P1 O5 112.40(15) 2_676 2_676
O1 P1 C18 107.47(15) 2_676 .
Tb2 O4 Tb1 112.70(9) . .
P1 O4 Tb1 101.50(12) . .
P1 O4 Tb2 125.96(13) . .
C16 O2 Tb1 124.7(2) . .
Tb2 O5 Tb1 118.02(10) . 2_676
P1 O5 Tb1 95.43(11) 2_676 2_676
P1 O5 Tb2 131.94(14) 2_676 .
C1 O6 Tb2 133.7(2) . .
Tb1 O3 H3 120.1(16) . .
C1AA O3 Tb1 132.8(5) . .
C1AA O3 H3 106.6(15) . .
P1 O1 Tb1 143.37(15) 2_676 .
Tb2 O9 Tb1 112.05(9) . .
C9 O9 Tb1 119.2(2) . .
C9 O9 Tb2 124.4(2) . .
C1 O15 Tb1 136.6(2) . 2_676
Tb2 O11 H11 119(4) . .
C3 O11 Tb2 126.0(2) . .
C3 O11 H11 102(4) . .
N2 N8 Tb1 121.5(2) . .
C10 N8 Tb1 123.6(2) . .
C10 N8 N2 114.7(3) . .
C4 N10 Tb2 118.2(2) . .
C8 N10 Tb2 124.2(2) . .
C8 N10 C4 117.5(3) . .
O11 C3 H3A 110.0 . .
O11 C3 H3B 110.0 . .
O11 C3 C29 108.6(3) . .
H3A C3 H3B 108.4 . .
C29 C3 H3A 110.0 . .
C29 C3 H3B 110.0 . .
N8 N2 H2 124.8 . .
C9 N2 N8 110.4(3) . .
C9 N2 H2 124.8 . .
C17 N7 Tb1 117.8(2) . .
C11 N7 Tb1 123.2(2) . .
C11 N7 C17 118.5(3) . .
O6 C1 C22 114.4(3) . .
O15 C1 O6 130.5(4) . .
O15 C1 C22 115.0(3) . .
O9 C9 N2 125.7(3) . .
O9 C9 C4 117.7(3) . .
N2 C9 C4 116.5(3) . .
N7 C17 C12 123.0(3) . .
N7 C17 C16 115.3(3) . .
C12 C17 C16 121.8(3) . .
C14 C12 C17 117.9(3) . .
C13 C12 C17 116.4(3) . .
C13 C12 C14 125.7(3) . .
O2 C16 C17 117.6(3) . .
O2 C16 C15 124.9(3) . .
C15 C16 C17 117.5(3) . .
N10 C4 C9 113.3(3) . .
N10 C4 C5 122.7(3) . .
C5 C4 C9 123.8(3) . .
C8 C7 H7 120.7 . .
C8 C7 C6 118.7(4) . .
C6 C7 H7 120.7 . .
C4 C5 H5 120.4 . .
C4 C5 C6 119.3(4) . .
C6 C5 H5 120.4 . .
C16 C15 H15 119.5 . .
C16 C15 C24 121.0(4) . .
C24 C15 H15 119.5 . .
N8 C10 H10 121.5 . .
N8 C10 C11 117.1(3) . .
C11 C10 H10 121.5 . .
N7 C11 C10 114.5(3) . .
N7 C11 C23 122.8(3) . .
C23 C11 C10 122.6(3) . .
C12 C14 H14 120.0 . .
C24 C14 C12 120.0(3) . .
C24 C14 H14 120.0 . .
N10 C8 C7 123.0(3) . .
N10 C8 C28 115.8(3) . .
C7 C8 C28 121.1(3) . .
C12 C13 H13 119.8 . .
C23 C13 C12 120.3(3) . .
C23 C13 H13 119.8 . .
C7 C6 H6 120.6 . .
C5 C6 C7 118.7(4) . .
C5 C6 H6 120.6 . .
Tb2 O17 H17 125.9(16) . .
C26 O17 Tb2 118.0(2) . .
C26 O17 H17 106.3(15) . .
C28 N1 Tb2 112.7(2) . .
C28 N1 C27 109.1(3) . .
C29 N1 Tb2 107.0(2) . .
C29 N1 C28 108.4(3) . .
C29 N1 C27 111.9(3) . .
C27 N1 Tb2 107.9(2) . .
C19 C18 P1 111.2(3) . .
C19 C18 C21 109.6(4) . .
C19 C18 C20 109.9(3) . .
C21 C18 P1 108.5(3) . .
C20 C18 P1 108.4(3) . .
C20 C18 C21 109.1(3) . .
C15 C24 H24 119.0 . .
C14 C24 C15 122.0(4) . .
C14 C24 H24 119.0 . .
C11 C23 H23 120.6 . .
C13 C23 C11 118.8(3) . .
C13 C23 H23 120.6 . .
C18 C19 H19A 109.5 . .
C18 C19 H19B 109.5 . .
C18 C19 H19C 109.5 . .
H19A C19 H19B 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
C8 C28 H28A 109.3 . .
C8 C28 H28B 109.3 . .
N1 C28 C8 111.5(3) . .
N1 C28 H28A 109.3 . .
N1 C28 H28B 109.3 . .
H28A C28 H28B 108.0 . .
F1 C22 C1 114.3(3) . .
F1 C22 F3 106.5(4) . .
F3 C22 C1 109.5(3) . .
F2 C22 F1 107.6(4) . .
F2 C22 C1 112.9(4) . .
F2 C22 F3 105.4(4) . .
C18 C21 H21A 109.5 . .
C18 C21 H21B 109.5 . .
C18 C21 H21C 109.5 . .
H21A C21 H21B 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C3 C29 H29A 109.6 . .
C3 C29 H29B 109.6 . .
N1 C29 C3 110.5(3) . .
N1 C29 H29A 109.6 . .
N1 C29 H29B 109.6 . .
H29A C29 H29B 108.1 . .
C18 C20 H20A 109.5 . .
C18 C20 H20B 109.5 . .
C18 C20 H20C 109.5 . .
H20A C20 H20B 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
O17 C26 H26A 109.9 . .
O17 C26 H26B 109.9 . .
O17 C26 C27 108.8(4) . .
H26A C26 H26B 108.3 . .
C27 C26 H26A 109.9 . .
C27 C26 H26B 109.9 . .
N1 C27 C26 112.8(4) . .
N1 C27 H27A 109.0 . .
N1 C27 H27B 109.0 . .
C26 C27 H27A 109.0 . .
C26 C27 H27B 109.0 . .
H27A C27 H27B 107.8 . .
O3 C1AA H1AA 109.5 . .
O3 C1AA H1AB 109.5 . .
O3 C1AA H1AC 109.5 . .
H1AA C1AA H1AB 109.5 . .
H1AA C1AA H1AC 109.5 . .
H1AB C1AA H1AC 109.5 . .
H1AD O1AA H1AE 104.5 . .
Tb1 O0AA H0AA 112.4 . .
Tb1 O0AA H0AB 111.2 . .
H0AA O0AA H0AB 103.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O4 2.494(2) .
Tb1 O2 2.359(2) .
Tb1 O5 2.647(2) 2_676
Tb1 O3 2.363(10) .
Tb1 O1 2.266(2) .
Tb1 O9 2.530(2) .
Tb1 O15 2.413(3) 2_676
Tb1 N8 2.554(3) .
Tb1 N7 2.557(3) .
Tb1 O0AA 2.53(5) .
Tb2 O4 2.393(2) .
Tb2 O5 2.300(3) .
Tb2 O6 2.356(2) .
Tb2 O9 2.374(2) .
Tb2 O11 2.405(3) .
Tb2 N10 2.570(3) .
Tb2 O17 2.356(3) .
Tb2 N1 2.679(3) .
P1 O4 1.551(3) .
P1 O5 1.545(3) 2_676
P1 O1 1.507(3) 2_676
P1 C18 1.814(4) .
O2 C16 1.326(4) .
O6 C1 1.254(4) .
O3 H3 0.869(9) .
O3 C1AA 1.442(13) .
O9 C9 1.287(4) .
O15 C1 1.222(5) .
O11 H11 0.77(5) .
O11 C3 1.436(4) .
N8 N2 1.389(4) .
N8 C10 1.284(4) .
F1 C22 1.318(5) .
N10 C4 1.347(5) .
N10 C8 1.338(5) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C3 C29 1.524(6) .
N2 H2 0.8800 .
N2 C9 1.312(5) .
N7 C17 1.348(5) .
N7 C11 1.324(5) .
C1 C22 1.541(5) .
C9 C4 1.483(5) .
C17 C12 1.426(5) .
C17 C16 1.435(5) .
C12 C14 1.415(5) .
C12 C13 1.408(5) .
C16 C15 1.372(5) .
C4 C5 1.375(5) .
C7 H7 0.9500 .
C7 C8 1.381(5) .
C7 C6 1.385(5) .
C5 H5 0.9500 .
C5 C6 1.376(5) .
C15 H15 0.9500 .
C15 C24 1.416(5) .
C10 H10 0.9500 .
C10 C11 1.459(5) .
C11 C23 1.411(5) .
C14 H14 0.9500 .
C14 C24 1.361(5) .
C8 C28 1.504(5) .
C13 H13 0.9500 .
C13 C23 1.365(5) .
C6 H6 0.9500 .
O17 H17 0.883(9) .
O17 C26 1.440(5) .
N1 C28 1.479(5) .
N1 C29 1.462(5) .
N1 C27 1.483(5) .
C18 C19 1.525(5) .
C18 C21 1.529(5) .
C18 C20 1.526(6) .
F3 C22 1.341(5) .
F2 C22 1.315(5) .
C24 H24 0.9500 .
C23 H23 0.9500 .
C19 H19A 0.9800 .
C19 H19B 0.9800 .
C19 H19C 0.9800 .
C28 H28A 0.9900 .
C28 H28B 0.9900 .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
C29 H29A 0.9900 .
C29 H29B 0.9900 .
C20 H20A 0.9800 .
C20 H20B 0.9800 .
C20 H20C 0.9800 .
C26 H26A 0.9900 .
C26 H26B 0.9900 .
C26 C27 1.494(6) .
C27 H27A 0.9900 .
C27 H27B 0.9900 .
C1AA H1AA 0.9800 .
C1AA H1AB 0.9800 .
C1AA H1AC 0.9800 .
O1AA H1AD 0.8700 .
O1AA H1AE 0.8699 .
O0AA H0AA 0.8948 .
O0AA H0AB 0.8928 .
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
O11 H11 O2 0.77(5) 1.86(5) 2.625(4) 174(5) 2_676 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
Tb1 O2 C16 C17 0.3(5) .
Tb1 O2 C16 C15 178.2(3) .
Tb1 O9 C9 N2 10.0(5) .
Tb1 O9 C9 C4 -173.2(2) .
Tb1 O15 C1 O6 -34.2(6) 2_676
Tb1 O15 C1 C22 149.5(3) 2_676
Tb1 N8 N2 C9 -15.8(4) .
Tb1 N8 C10 C11 4.2(5) .
Tb1 N7 C17 C12 -175.3(3) .
Tb1 N7 C17 C16 3.8(4) .
Tb1 N7 C11 C10 -8.1(5) .
Tb1 N7 C11 C23 174.2(3) .
Tb2 O6 C1 O15 -11.4(6) .
Tb2 O6 C1 C22 165.0(2) .
Tb2 O9 C9 N2 164.6(3) .
Tb2 O9 C9 C4 -18.6(4) .
Tb2 O11 C3 C29 -16.7(4) .
Tb2 N10 C4 C9 3.6(4) .
Tb2 N10 C4 C5 179.3(3) .
Tb2 N10 C8 C7 -178.6(3) .
Tb2 N10 C8 C28 2.8(5) .
Tb2 O17 C26 C27 51.3(4) .
Tb2 N1 C28 C8 41.3(4) .
Tb2 N1 C29 C3 52.9(3) .
Tb2 N1 C27 C26 32.7(4) .
O4 P1 C18 C19 51.2(3) .
O4 P1 C18 C21 -69.5(3) .
O4 P1 C18 C20 172.1(3) .
O2 C16 C15 C24 -177.0(4) .
O5 P1 O4 Tb1 8.95(15) 2_676
O5 P1 O4 Tb2 -120.41(16) 2_676
O5 P1 C18 C19 -63.3(3) 2_676
O5 P1 C18 C21 176.0(3) 2_676
O5 P1 C18 C20 57.6(3) 2_676
O6 C1 C22 F1 29.3(5) .
O6 C1 C22 F3 -90.1(4) .
O6 C1 C22 F2 152.8(4) .
O1 P1 O4 Tb1 132.04(13) 2_676
O1 P1 O4 Tb2 2.7(2) 2_676
O1 P1 C18 C19 174.5(3) 2_676
O1 P1 C18 C21 53.9(3) 2_676
O1 P1 C18 C20 -64.5(3) 2_676
O9 C9 C4 N10 8.5(5) .
O9 C9 C4 C5 -167.0(4) .
O15 C1 C22 F1 -153.7(4) .
O15 C1 C22 F3 86.9(4) .
O15 C1 C22 F2 -30.3(5) .
O11 C3 C29 N1 -28.1(4) .
N8 N2 C9 O9 3.7(5) .
N8 N2 C9 C4 -173.2(3) .
N8 C10 C11 N7 2.5(5) .
N8 C10 C11 C23 -179.8(4) .
N10 C4 C5 C6 -1.0(6) .
N10 C8 C28 N1 -30.1(5) .
N2 N8 C10 C11 -171.7(3) .
N2 C9 C4 N10 -174.4(3) .
N2 C9 C4 C5 10.1(5) .
N7 C17 C12 C14 -179.5(3) .
N7 C17 C12 C13 0.9(6) .
N7 C17 C16 O2 -2.8(5) .
N7 C17 C16 C15 179.2(3) .
N7 C11 C23 C13 0.5(6) .
C9 C4 C5 C6 174.2(4) .
C17 N7 C11 C10 179.5(3) .
C17 N7 C11 C23 1.8(6) .
C17 C12 C14 C24 -0.4(6) .
C17 C12 C13 C23 1.5(6) .
C17 C16 C15 C24 0.8(6) .
C12 C17 C16 O2 176.3(3) .
C12 C17 C16 C15 -1.8(6) .
C12 C14 C24 C15 -0.5(6) .
C12 C13 C23 C11 -2.2(6) .
C16 C17 C12 C14 1.5(5) .
C16 C17 C12 C13 -178.1(3) .
C16 C15 C24 C14 0.2(6) .
C4 N10 C8 C7 -1.6(6) .
C4 N10 C8 C28 179.8(3) .
C4 C5 C6 C7 -0.6(6) .
C7 C8 C28 N1 151.2(4) .
C10 N8 N2 C9 160.3(3) .
C10 C11 C23 C13 -177.0(4) .
C11 N7 C17 C12 -2.5(6) .
C11 N7 C17 C16 176.6(3) .
C14 C12 C13 C23 -178.2(4) .
C8 N10 C4 C9 -173.5(3) .
C8 N10 C4 C5 2.1(6) .
C8 C7 C6 C5 1.1(6) .
C13 C12 C14 C24 179.2(4) .
C6 C7 C8 N10 0.1(6) .
C6 C7 C8 C28 178.6(4) .
O17 C26 C27 N1 -54.9(5) .
C18 P1 O4 Tb1 -108.09(15) .
C18 P1 O4 Tb2 122.54(18) .
C28 N1 C29 C3 -68.8(4) .
C28 N1 C27 C26 155.4(4) .
C29 N1 C28 C8 159.5(3) .
C29 N1 C27 C26 -84.7(4) .
C27 N1 C28 C8 -78.5(4) .
C27 N1 C29 C3 170.9(3) .
