# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2012


data_global

_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222
#TrackingRef '- CCDC-861035.cif'

_publ_contact_author             'Dr. Simon M. Humphrey'

_publ_contact_author_email       smh@cm.utexas.edu
loop_
_publ_author_name
'Ilich A. Ibarra'
'Travis W. Hesterberg'
'Bradley J. Holliday'
'Vincent M. Lynch'
'Simon M. Humphrey'
_publ_contact_author_name        'Dr. Simon M. Humphrey'

data_sh11018
_database_code_depnum_ccdc_archive 'CCDC 861035'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H14 O7 P Tb, C3 H7 N O, 2(H2 O)'
_chemical_formula_sum            'C24 H25 N O10 P Tb'
_chemical_formula_weight         671.29

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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pccn

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   27.185(5)
_cell_length_b                   12.100(2)
_cell_length_c                   20.605(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6778(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    15879
_cell_measurement_theta_min      1.5
_cell_measurement_theta_max      25.0

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2640
_exptl_absorpt_coefficient_mu    2.177
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.334
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
SADABS: Area-Detector Absorption Correction. (1996)
Siemens Industrial Automation, Inc.: Madison, WI.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+ CCD'
_diffrn_measurement_method       \w-scans
_diffrn_reflns_number            60180
_diffrn_reflns_av_R_equivalents  0.1849
_diffrn_reflns_av_sigmaI/netI    0.1178
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.59
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5944
_reflns_number_gt                3576
_reflns_threshold_expression     >2sigma(I)

_publ_section_references         
;
Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C.,
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97.
(1999) J. Appl. Cryst. 32, 115-119.

Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. An Integrated System
of Windows Programs for the Solution, Refinement and Analysis of
Single Crystal X-ray Diffraction Data.

Sheldrick, G. M. (2008). SHELXL-97. Acta Cryst., A64, 112-122.

Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201.

Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht
University, Utrecht, The Netherlands.
;
_publ_section_acknowledgements   
;
The data were collected using instrumentation purchased with funds provided
by the National Science Foundation Grant No. 0741973.
;

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'

_computing_structure_solution    
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C.,
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_computing_structure_refinement  'XL SHELXTL/PC, Siemens Analytical'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

Solvent molecules were refined with free variables applied to determine
the site occupancies, which were set to 1.0 or 0.5 in the final
refinement cycles. SQUEEZE was used to remove the effects due to
residual peaks from disordered solvent.
The contributions to the
scattering factors due to these disordered solvent molecules were removed
by use of the utility SQUEEZE (Sluis and Spek, 1990) in PLATON98
(Spek, 1998). PLATON98 was used as incorporated in WinGX (Farrugia, 1999).
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0730P)^2^+21.9981P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5944
_refine_ls_number_parameters     305
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.1513
_refine_ls_R_factor_gt           0.0795
_refine_ls_wR_factor_ref         0.1894
_refine_ls_wR_factor_gt          0.1603
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.89206(12) 0.1218(2) 0.09595(14) 0.0286(7) Uani 1 1 d . . .
Tb1 Tb 0.57143(2) 0.11089(4) 0.02225(3) 0.0295(2) Uani 1 1 d . . .
O1P O 0.9202(3) 0.2079(5) 0.0592(4) 0.0306(19) Uani 1 1 d . . .
O1 O 0.9176(3) -0.4205(6) 0.0360(4) 0.047(3) Uani 1 1 d . . .
O2 O 0.9904(3) -0.3655(6) 0.0024(4) 0.042(2) Uani 1 1 d . . .
O3 O 0.9348(3) 0.0368(6) 0.4135(3) 0.042(2) Uani 1 1 d . . .
O4 O 0.9210(3) 0.2173(6) 0.4195(4) 0.036(2) Uani 1 1 d . . .
O5 O 0.6410(3) 0.0982(6) 0.0980(4) 0.036(2) Uani 1 1 d . . .
O6 O 0.6566(3) 0.1020(7) -0.0078(3) 0.037(2) Uani 1 1 d . . .
O7 O 0.5251(4) 0.0754(7) 0.1191(4) 0.049(3) Uani 1 1 d . . .
C1 C 0.9085(4) -0.0156(9) 0.0709(5) 0.027(3) Uani 1 1 d . . .
C2 C 0.8734(5) -0.0969(9) 0.0657(7) 0.053(4) Uani 1 1 d . . .
H2A H 0.8396 -0.0795 0.0714 0.064 Uiso 1 1 calc R . .
C3 C 0.8877(5) -0.2059(10) 0.0519(8) 0.057(4) Uani 1 1 d . . .
H3A H 0.8638 -0.2630 0.0505 0.069 Uiso 1 1 calc R . .
C4 C 0.9350(4) -0.2298(9) 0.0408(5) 0.029(3) Uiso 1 1 d . . .
C5 C 0.9708(5) -0.1480(9) 0.0442(6) 0.044(3) Uani 1 1 d . . .
H5A H 1.0044 -0.1651 0.0371 0.053 Uiso 1 1 calc R . .
C6 C 0.9565(5) -0.0426(9) 0.0580(6) 0.038(3) Uani 1 1 d . . .
H6A H 0.9807 0.0141 0.0586 0.045 Uiso 1 1 calc R . .
C7 C 0.9492(4) -0.3471(9) 0.0254(6) 0.032(3) Uani 1 1 d . . .
C8 C 0.9039(5) 0.1252(8) 0.1820(5) 0.032(3) Uani 1 1 d . . .
C9 C 0.9105(6) 0.0262(11) 0.2156(6) 0.058(4) Uani 1 1 d . . .
H9A H 0.9103 -0.0423 0.1930 0.070 Uiso 1 1 calc R . .
C10 C 0.9173(6) 0.0287(10) 0.2824(6) 0.051(4) Uani 1 1 d . . .
H10H H 0.9210 -0.0386 0.3057 0.062 Uiso 1 1 calc R . .
C11 C 0.9189(5) 0.1293(9) 0.3155(5) 0.036(3) Uani 1 1 d . . .
C12 C 0.9152(6) 0.2261(10) 0.2807(7) 0.060(5) Uani 1 1 d . . .
H12A H 0.9168 0.2954 0.3023 0.072 Uiso 1 1 calc R . .
C13 C 0.9090(6) 0.2216(9) 0.2129(6) 0.048(4) Uani 1 1 d . . .
H13A H 0.9084 0.2883 0.1886 0.058 Uiso 1 1 calc R . .
C14 C 0.9257(5) 0.1309(9) 0.3869(5) 0.033(3) Uani 1 1 d . . .
C15 C 0.8275(5) 0.1265(8) 0.0856(5) 0.033(3) Uani 1 1 d . . .
C16 C 0.7930(5) 0.1179(10) 0.1374(6) 0.040(3) Uani 1 1 d . . .
H16A H 0.8048 0.1171 0.1808 0.048 Uiso 1 1 calc R . .
C17 C 0.7430(5) 0.1106(11) 0.1265(6) 0.045(3) Uani 1 1 d . . .
H17A H 0.7205 0.1073 0.1618 0.053 Uiso 1 1 calc R . .
C18 C 0.7264(4) 0.1082(9) 0.0630(5) 0.033(3) Uani 1 1 d . . .
C19 C 0.7589(5) 0.1151(11) 0.0114(6) 0.045(3) Uani 1 1 d . . .
H19A H 0.7470 0.1125 -0.0319 0.054 Uiso 1 1 calc R . .
C20 C 0.8094(4) 0.1259(9) 0.0235(6) 0.037(3) Uani 1 1 d . . .
H20A H 0.8315 0.1329 -0.0120 0.044 Uiso 1 1 calc R . .
C21 C 0.6719(4) 0.1013(9) 0.0508(6) 0.032(3) Uani 1 1 d . . .
O100 O 0.5536(8) 0.016(2) 0.2425(11) 0.210(9) Uiso 1 1 d D . .
N100 N 0.5589(10) -0.103(2) 0.3345(13) 0.35(3) Uiso 1 1 d D . .
C102 C 0.5451(10) -0.204(2) 0.3593(11) 0.137(9) Uiso 1 1 d D . .
H10A H 0.5255 -0.2439 0.3269 0.205 Uiso 1 1 calc R . .
H10B H 0.5253 -0.1928 0.3986 0.205 Uiso 1 1 calc R . .
H10C H 0.5745 -0.2470 0.3700 0.205 Uiso 1 1 calc R . .
C101 C 0.5850(15) -0.027(3) 0.3719(18) 0.30(2) Uiso 1 1 d D . .
H10D H 0.5917 0.0390 0.3461 0.453 Uiso 1 1 calc R . .
H10E H 0.6161 -0.0606 0.3858 0.453 Uiso 1 1 calc R . .
H10F H 0.5655 -0.0072 0.4101 0.453 Uiso 1 1 calc R . .
C100 C 0.5448(11) -0.081(3) 0.2720(13) 0.31(3) Uiso 1 1 d D . .
H10G H 0.5280 -0.1368 0.2485 0.374 Uiso 1 1 calc R . .
O50 O 0.3307(14) 0.119(3) 0.0903(16) 0.148(12) Uiso 0.50 1 d P . .
O51 O 0.6620(17) 0.896(3) 0.187(2) 0.193(17) Uiso 0.50 1 d P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.0332(19) 0.0176(14) 0.0351(16) -0.0027(13) -0.0045(14) 0.0034(14)
Tb1 0.0320(3) 0.0195(3) 0.0369(3) 0.0030(3) 0.0004(3) -0.0021(3)
O1P 0.029(5) 0.018(4) 0.045(4) 0.000(3) -0.003(4) 0.000(3)
O1 0.065(7) 0.016(4) 0.061(6) -0.007(4) 0.019(5) -0.014(4)
O2 0.034(5) 0.024(4) 0.067(5) -0.021(4) 0.004(4) 0.000(4)
O3 0.062(7) 0.033(5) 0.031(4) 0.007(4) -0.005(4) 0.006(5)
O4 0.035(6) 0.024(4) 0.050(5) 0.001(4) 0.006(4) 0.005(4)
O5 0.038(5) 0.031(5) 0.040(5) -0.001(4) 0.000(4) -0.002(4)
O6 0.043(5) 0.048(5) 0.021(4) -0.001(4) -0.005(4) 0.013(4)
O7 0.060(7) 0.052(6) 0.035(5) -0.003(4) 0.013(4) -0.008(5)
C1 0.014(6) 0.021(6) 0.044(7) -0.003(5) -0.015(5) -0.001(5)
C2 0.034(8) 0.015(6) 0.111(11) -0.024(7) 0.018(8) -0.003(6)
C3 0.024(8) 0.023(7) 0.125(13) -0.014(7) 0.015(8) -0.001(6)
C5 0.036(8) 0.020(6) 0.076(9) -0.011(6) 0.013(7) -0.012(6)
C6 0.037(9) 0.020(6) 0.057(8) 0.000(6) -0.009(7) -0.007(6)
C7 0.026(7) 0.030(6) 0.039(7) -0.015(6) 0.013(6) 0.006(5)
C8 0.051(8) 0.011(5) 0.036(6) -0.002(5) -0.007(6) 0.007(5)
C9 0.093(13) 0.036(8) 0.046(8) -0.016(6) -0.019(8) 0.001(8)
C10 0.081(13) 0.028(7) 0.044(8) 0.014(6) -0.001(7) 0.011(7)
C11 0.047(9) 0.032(7) 0.030(6) 0.007(5) -0.014(6) 0.016(6)
C12 0.092(14) 0.019(7) 0.069(10) -0.003(6) -0.007(9) -0.011(7)
C13 0.091(12) 0.021(6) 0.032(7) 0.012(5) -0.016(7) -0.007(7)
C14 0.028(7) 0.035(7) 0.036(6) 0.011(5) -0.008(6) 0.024(6)
C15 0.043(8) 0.016(6) 0.041(7) -0.005(5) -0.009(6) -0.005(5)
C16 0.041(8) 0.035(7) 0.043(7) -0.003(6) -0.002(6) 0.006(7)
C17 0.044(9) 0.047(8) 0.043(8) -0.003(7) 0.001(6) 0.007(7)
C18 0.032(7) 0.030(6) 0.037(7) -0.006(6) 0.003(6) -0.003(6)
C19 0.045(9) 0.053(8) 0.037(7) -0.017(7) -0.013(6) 0.018(7)
C20 0.035(7) 0.039(7) 0.035(6) 0.003(6) 0.001(6) 0.012(6)
C21 0.029(7) 0.022(6) 0.046(7) 0.009(6) -0.002(6) 0.003(6)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 O1P 1.497(8) . ?
P1 C15 1.770(13) . ?
P1 C1 1.797(11) . ?
P1 C8 1.802(11) . ?
Tb1 O2 2.278(9) 6_565 ?
Tb1 O1P 2.333(7) 2_655 ?
Tb1 O1 2.340(7) 2_645 ?
Tb1 O7 2.398(8) . ?
Tb1 O6 2.399(8) . ?
Tb1 O3 2.420(7) 8_755 ?
Tb1 O5 2.457(8) . ?
Tb1 O4 2.486(7) 8_755 ?
Tb1 C21 2.797(12) . ?
Tb1 C14 2.800(11) 8_755 ?
O1P Tb1 2.333(7) 2_655 ?
O1 C7 1.255(14) . ?
O1 Tb1 2.340(7) 2_645 ?
O2 C7 1.238(13) . ?
O2 Tb1 2.278(9) 6_655 ?
O3 C14 1.289(12) . ?
O3 Tb1 2.420(7) 8_756 ?
O4 C14 1.249(12) . ?
O4 Tb1 2.486(7) 8_756 ?
O5 C21 1.287(14) . ?
O6 C21 1.277(13) . ?
C1 C6 1.372(16) . ?
C1 C2 1.375(15) . ?
C2 C3 1.405(15) . ?
C2 H2A 0.9500 . ?
C3 C4 1.337(17) . ?
C3 H3A 0.9500 . ?
C4 C5 1.388(15) . ?
C4 C7 1.504(15) . ?
C5 C6 1.362(16) . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9500 . ?
C8 C13 1.336(15) . ?
C8 C9 1.395(16) . ?
C9 C10 1.388(17) . ?
C9 H9A 0.9500 . ?
C10 C11 1.397(16) . ?
C10 H10H 0.9500 . ?
C11 C12 1.378(16) . ?
C11 C14 1.482(15) . ?
C12 C13 1.409(17) . ?
C12 H12A 0.9500 . ?
C13 H13A 0.9500 . ?
C14 Tb1 2.800(11) 8_756 ?
C15 C20 1.371(15) . ?
C15 C16 1.425(17) . ?
C16 C17 1.381(17) . ?
C16 H16A 0.9500 . ?
C17 C18 1.385(16) . ?
C17 H17A 0.9500 . ?
C18 C19 1.384(17) . ?
C18 C21 1.504(16) . ?
C19 C20 1.403(17) . ?
C19 H19A 0.9500 . ?
C20 H20A 0.9500 . ?
O100 C100 1.34(2) . ?
N100 C100 1.37(2) . ?
N100 C102 1.378(19) . ?
N100 C101 1.39(2) . ?
C102 H10A 0.9800 . ?
C102 H10B 0.9800 . ?
C102 H10C 0.9800 . ?
C101 H10D 0.9800 . ?
C101 H10E 0.9800 . ?
C101 H10F 0.9800 . ?
C100 H10G 0.9500 . ?

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
O1P P1 C15 115.0(5) . . ?
O1P P1 C1 111.8(5) . . ?
C15 P1 C1 104.0(5) . . ?
O1P P1 C8 113.0(5) . . ?
C15 P1 C8 107.2(6) . . ?
C1 P1 C8 105.0(5) . . ?
O2 Tb1 O1P 92.8(3) 6_565 2_655 ?
O2 Tb1 O1 105.9(3) 6_565 2_645 ?
O1P Tb1 O1 150.9(3) 2_655 2_645 ?
O2 Tb1 O7 72.6(3) 6_565 . ?
O1P Tb1 O7 87.0(3) 2_655 . ?
O1 Tb1 O7 77.9(3) 2_645 . ?
O2 Tb1 O6 151.8(3) 6_565 . ?
O1P Tb1 O6 91.8(3) 2_655 . ?
O1 Tb1 O6 82.2(3) 2_645 . ?
O7 Tb1 O6 135.5(3) . . ?
O2 Tb1 O3 76.8(3) 6_565 8_755 ?
O1P Tb1 O3 131.1(2) 2_655 8_755 ?
O1 Tb1 O3 75.9(3) 2_645 8_755 ?
O7 Tb1 O3 131.9(3) . 8_755 ?
O6 Tb1 O3 79.2(3) . 8_755 ?
O2 Tb1 O5 153.3(3) 6_565 . ?
O1P Tb1 O5 77.1(3) 2_655 . ?
O1 Tb1 O5 76.3(3) 2_645 . ?
O7 Tb1 O5 82.2(3) . . ?
O6 Tb1 O5 54.4(2) . . ?
O3 Tb1 O5 128.3(3) 8_755 . ?
O2 Tb1 O4 80.0(3) 6_565 8_755 ?
O1P Tb1 O4 77.5(2) 2_655 8_755 ?
O1 Tb1 O4 127.0(3) 2_645 8_755 ?
O7 Tb1 O4 147.6(3) . 8_755 ?
O6 Tb1 O4 74.0(3) . 8_755 ?
O3 Tb1 O4 53.8(3) 8_755 8_755 ?
O5 Tb1 O4 120.6(3) . 8_755 ?
O2 Tb1 C21 175.1(3) 6_565 . ?
O1P Tb1 C21 82.8(3) 2_655 . ?
O1 Tb1 C21 79.0(3) 2_645 . ?
O7 Tb1 C21 109.3(3) . . ?
O6 Tb1 C21 27.1(3) . . ?
O3 Tb1 C21 104.4(3) 8_755 . ?
O5 Tb1 C21 27.4(3) . . ?
O4 Tb1 C21 96.9(3) 8_755 . ?
O2 Tb1 C14 78.1(3) 6_565 8_755 ?
O1P Tb1 C14 104.0(3) 2_655 8_755 ?
O1 Tb1 C14 101.7(3) 2_645 8_755 ?
O7 Tb1 C14 149.2(3) . 8_755 ?
O6 Tb1 C14 73.7(3) . 8_755 ?
O3 Tb1 C14 27.4(3) 8_755 8_755 ?
O5 Tb1 C14 128.1(3) . 8_755 ?
O4 Tb1 C14 26.5(3) 8_755 8_755 ?
C21 Tb1 C14 100.7(4) . 8_755 ?
P1 O1P Tb1 150.3(5) . 2_655 ?
C7 O1 Tb1 126.1(8) . 2_645 ?
C7 O2 Tb1 169.7(8) . 6_655 ?
C14 O3 Tb1 93.0(7) . 8_756 ?
C14 O4 Tb1 90.9(6) . 8_756 ?
C21 O5 Tb1 91.2(7) . . ?
C21 O6 Tb1 94.1(7) . . ?
C6 C1 C2 118.3(11) . . ?
C6 C1 P1 120.9(8) . . ?
C2 C1 P1 120.8(9) . . ?
C1 C2 C3 119.7(12) . . ?
C1 C2 H2A 120.2 . . ?
C3 C2 H2A 120.2 . . ?
C4 C3 C2 120.3(12) . . ?
C4 C3 H3A 119.9 . . ?
C2 C3 H3A 119.9 . . ?
C3 C4 C5 120.7(11) . . ?
C3 C4 C7 119.0(10) . . ?
C5 C4 C7 120.3(11) . . ?
C6 C5 C4 118.6(12) . . ?
C6 C5 H5A 120.7 . . ?
C4 C5 H5A 120.7 . . ?
C5 C6 C1 122.3(11) . . ?
C5 C6 H6A 118.9 . . ?
C1 C6 H6A 118.9 . . ?
O2 C7 O1 123.9(10) . . ?
O2 C7 C4 118.9(10) . . ?
O1 C7 C4 117.2(10) . . ?
C13 C8 C9 120.0(11) . . ?
C13 C8 P1 120.5(8) . . ?
C9 C8 P1 119.5(8) . . ?
C10 C9 C8 119.4(11) . . ?
C10 C9 H9A 120.3 . . ?
C8 C9 H9A 120.3 . . ?
C9 C10 C11 120.5(11) . . ?
C9 C10 H10H 119.7 . . ?
C11 C10 H10H 119.7 . . ?
C12 C11 C10 119.0(11) . . ?
C12 C11 C14 120.9(10) . . ?
C10 C11 C14 120.1(10) . . ?
C11 C12 C13 119.5(11) . . ?
C11 C12 H12A 120.3 . . ?
C13 C12 H12A 120.3 . . ?
C8 C13 C12 121.3(11) . . ?
C8 C13 H13A 119.4 . . ?
C12 C13 H13A 119.4 . . ?
O4 C14 O3 122.1(10) . . ?
O4 C14 C11 122.2(9) . . ?
O3 C14 C11 115.7(10) . . ?
O4 C14 Tb1 62.6(6) . 8_756 ?
O3 C14 Tb1 59.6(5) . 8_756 ?
C11 C14 Tb1 172.1(9) . 8_756 ?
C20 C15 C16 117.7(12) . . ?
C20 C15 P1 117.9(10) . . ?
C16 C15 P1 124.0(9) . . ?
C17 C16 C15 122.0(12) . . ?
C17 C16 H16A 119.0 . . ?
C15 C16 H16A 119.0 . . ?
C16 C17 C18 118.4(12) . . ?
C16 C17 H17A 120.8 . . ?
C18 C17 H17A 120.8 . . ?
C17 C18 C19 121.2(12) . . ?
C17 C18 C21 118.6(11) . . ?
C19 C18 C21 120.2(11) . . ?
C18 C19 C20 119.6(11) . . ?
C18 C19 H19A 120.2 . . ?
C20 C19 H19A 120.2 . . ?
C15 C20 C19 121.1(12) . . ?
C15 C20 H20A 119.5 . . ?
C19 C20 H20A 119.5 . . ?
O6 C21 O5 120.1(11) . . ?
O6 C21 C18 118.6(11) . . ?
O5 C21 C18 121.3(11) . . ?
O6 C21 Tb1 58.8(6) . . ?
O5 C21 Tb1 61.4(6) . . ?
C18 C21 Tb1 173.9(8) . . ?
C100 N100 C102 116.4(17) . . ?
C100 N100 C101 122.4(17) . . ?
C102 N100 C101 121.1(17) . . ?
N100 C102 H10A 109.5 . . ?
N100 C102 H10B 109.5 . . ?
H10A C102 H10B 109.5 . . ?
N100 C102 H10C 109.5 . . ?
H10A C102 H10C 109.5 . . ?
H10B C102 H10C 109.5 . . ?
N100 C101 H10D 109.5 . . ?
N100 C101 H10E 109.5 . . ?
H10D C101 H10E 109.5 . . ?
N100 C101 H10F 109.5 . . ?
H10D C101 H10F 109.5 . . ?
H10E C101 H10F 109.5 . . ?
O100 C100 N100 123(2) . . ?
O100 C100 H10G 118.4 . . ?
N100 C100 H10G 118.4 . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.310
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.157

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.250 0.147 0.133 1070 308 ' '
2 0.750 -0.156 0.370 1070 306 ' '
_platon_squeeze_details          
;
;