# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 2031255'
_audit_update_record             
;
2020-09-10 deposited with the CCDC.	2020-12-14 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H15 Dy O9 P3'
_chemical_formula_sum            'C12 H15 Dy O9 P3'
_chemical_formula_weight         558.65

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.0836(8)
_cell_length_b                   9.4719(8)
_cell_length_c                   12.1265(10)
_cell_angle_alpha                67.642(2)
_cell_angle_beta                 70.658(2)
_cell_angle_gamma                64.713(2)
_cell_volume                     854.52(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6492
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      28.36

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.171
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             540
_exptl_absorpt_coefficient_mu    4.697
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4852
_exptl_absorpt_correction_T_max  0.6026
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12603
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0319
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.48
_diffrn_reflns_theta_max         28.47
_reflns_number_total             4246
_reflns_number_gt                3912
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0249P)²+0.0000P] where P=(Fo²+2Fc²)/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         4246
_refine_ls_number_parameters     226
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0222
_refine_ls_wR_factor_ref         0.0472
_refine_ls_wR_factor_gt          0.0460
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_refine_ls_shift/su_max          0.004
_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
Dy1 Dy 0.162620(14) 1.197223(14) 0.005759(9) 0.01817(5) Uani 1 1 d . . .
P1 P 0.49359(9) 1.06690(9) 0.15254(6) 0.02083(14) Uani 1 1 d . . .
P2 P 0.22736(9) 0.58397(8) 0.84507(6) 0.02198(15) Uani 1 1 d . . .
P3 P 0.05491(8) 0.83417(8) 0.17689(6) 0.01934(14) Uani 1 1 d . . .
C1 C 0.5010(4) 1.0575(4) 0.3015(2) 0.0276(6) Uani 1 1 d . . .
H1A H 0.6167 1.0368 0.3032 0.033 Uiso 1 1 calc R . .
H1B H 0.4313 1.1645 0.3170 0.033 Uiso 1 1 calc R . .
C2 C 0.4423(4) 0.9283(4) 0.4021(2) 0.0255(6) Uani 1 1 d . . .
C3 C 0.5540(4) 0.7760(4) 0.4474(2) 0.0317(7) Uani 1 1 d . . .
H3 H 0.6695 0.7519 0.4137 0.038 Uiso 1 1 calc R . .
C4 C 0.4986(4) 0.6590(4) 0.5414(2) 0.0335(7) Uani 1 1 d . . .
H4 H 0.5773 0.5555 0.5708 0.040 Uiso 1 1 calc R . .
C5 C 0.3324(4) 0.6888(4) 0.5934(2) 0.0290(6) Uani 1 1 d . . .
C6 C 0.2742(4) 0.5600(4) 0.6964(2) 0.0316(7) Uani 1 1 d . . .
H6A H 0.3615 0.4525 0.6950 0.038 Uiso 1 1 calc R . .
H6B H 0.1736 0.5597 0.6815 0.038 Uiso 1 1 calc R . .
C7 C 0.2207(4) 0.8406(4) 0.5481(3) 0.0332(7) Uani 1 1 d . . .
H7 H 0.1055 0.8649 0.5829 0.040 Uiso 1 1 calc R . .
C8 C 0.2749(4) 0.9571(4) 0.4529(3) 0.0315(7) Uani 1 1 d . . .
H8 H 0.1957 1.0591 0.4217 0.038 Uiso 1 1 calc R . .
C9 C 0.1797(3) 0.6797(4) 0.2837(2) 0.0273(6) Uani 1 1 d . . .
H9A H 0.2713 0.6018 0.2414 0.033 Uiso 1 1 calc R . .
H9B H 0.2304 0.7312 0.3113 0.033 Uiso 1 1 calc R . .
C10 C 0.0859(3) 0.5857(3) 0.3949(2) 0.0241(6) Uani 1 1 d . . .
C11 C 0.0031(4) 0.6446(4) 0.4948(3) 0.0357(7) Uani 1 1 d . . .
H11 H 0.0039 0.7455 0.4928 0.043 Uiso 1 1 calc R . .
C12 C 0.0817(4) 0.4394(4) 0.4016(3) 0.0347(7) Uani 1 1 d . . .
H12 H 0.1376 0.3951 0.3344 0.042 Uiso 1 1 calc R . .
O1 O 0.3152(2) 1.1227(3) 0.14381(16) 0.0291(4) Uani 1 1 d . . .
O2 O 0.5697(3) 1.2050(2) 0.06549(17) 0.0322(5) Uani 1 1 d . . .
H2A H 0.6507 1.1697 0.0208 0.048 Uiso 1 1 d R . .
O3 O 0.6055(2) 0.9108(2) 0.12060(16) 0.0271(4) Uani 1 1 d . . .
O4 O 0.3952(3) 0.5800(3) 0.8569(2) 0.0386(5) Uani 1 1 d . . .
H4A H 0.3963 0.6485 0.8758 0.058 Uiso 1 1 d R . .
O5 O 0.1843(3) 0.4405(2) 0.93586(17) 0.0306(5) Uani 1 1 d . . .
O6 O 0.0896(2) 0.7449(2) 0.85550(17) 0.0282(4) Uani 1 1 d . . .
O7 O 0.1586(2) 0.9321(2) 0.07970(15) 0.0246(4) Uani 1 1 d . . .
O8 O -0.0887(3) 0.9480(2) 0.25216(18) 0.0363(5) Uani 1 1 d . . .
H8A H -0.0906 1.0510 0.2236 0.054 Uiso 1 1 d R . .
O9 O -0.0149(3) 0.7570(2) 0.12955(17) 0.0311(5) Uani 1 1 d . . .


_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
Dy1 O5 2.2040(19) 1_564 ?
Dy1 O1 2.2412(18) . ?
Dy1 O3 2.2458(18) 2_675 ?
Dy1 O9 2.2586(19) 2_575 ?
Dy1 O7 2.3351(18) . ?
Dy1 O6 2.3358(18) 2_576 ?
P1 O1 1.502(2) . ?
P1 O3 1.504(2) . ?
P1 O2 1.595(2) . ?
P1 C1 1.797(3) . ?
P2 O5 1.4976(19) . ?
P2 O6 1.522(2) . ?
P2 O4 1.561(2) . ?
P2 C6 1.790(3) . ?
P3 O9 1.491(2) . ?
P3 O7 1.5223(17) . ?
P3 O8 1.567(2) . ?
P3 C9 1.794(3) . ?
C1 C2 1.503(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C8 1.385(4) . ?
C2 C3 1.389(4) . ?
C3 C4 1.384(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.378(4) . ?
C4 H4 0.9500 . ?
C5 C7 1.386(4) . ?
C5 C6 1.510(4) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.383(4) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.520(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C12 1.374(4) . ?
C10 C11 1.377(4) . ?
C11 C12 1.388(4) 2_566 ?
C11 H11 0.9500 . ?
C12 C11 1.388(4) 2_566 ?
C12 H12 0.9500 . ?
O2 H2A 0.7809 . ?
O3 Dy1 2.2458(18) 2_675 ?
O4 H4A 0.7716 . ?
O5 Dy1 2.2040(19) 1_546 ?
O6 Dy1 2.3358(18) 2_576 ?
O8 H8A 0.8965 . ?
O9 Dy1 2.2586(19) 2_575 ?

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
O5 Dy1 O1 90.62(8) 1_564 . ?
O5 Dy1 O3 94.18(7) 1_564 2_675 ?
O1 Dy1 O3 89.32(7) . 2_675 ?
O5 Dy1 O9 95.38(7) 1_564 2_575 ?
O1 Dy1 O9 173.72(7) . 2_575 ?
O3 Dy1 O9 88.38(7) 2_675 2_575 ?
O5 Dy1 O7 176.17(7) 1_564 . ?
O1 Dy1 O7 86.71(7) . . ?
O3 Dy1 O7 83.06(6) 2_675 . ?
O9 Dy1 O7 87.21(7) 2_575 . ?
O5 Dy1 O6 98.62(7) 1_564 2_576 ?
O1 Dy1 O6 93.62(7) . 2_576 ?
O3 Dy1 O6 166.82(7) 2_675 2_576 ?
O9 Dy1 O6 87.33(7) 2_575 2_576 ?
O7 Dy1 O6 84.29(6) . 2_576 ?
O1 P1 O3 115.74(12) . . ?
O1 P1 O2 109.26(12) . . ?
O3 P1 O2 107.83(11) . . ?
O1 P1 C1 108.93(12) . . ?
O3 P1 C1 111.37(13) . . ?
O2 P1 C1 102.91(12) . . ?
O5 P2 O6 112.46(11) . . ?
O5 P2 O4 110.49(13) . . ?
O6 P2 O4 110.93(12) . . ?
O5 P2 C6 107.96(13) . . ?
O6 P2 C6 111.52(13) . . ?
O4 P2 C6 103.06(13) . . ?
O9 P3 O7 114.79(11) . . ?
O9 P3 O8 110.12(12) . . ?
O7 P3 O8 108.43(11) . . ?
O9 P3 C9 109.17(13) . . ?
O7 P3 C9 108.82(12) . . ?
O8 P3 C9 105.06(13) . . ?
C2 C1 P1 113.71(19) . . ?
C2 C1 H1A 108.8 . . ?
P1 C1 H1A 108.8 . . ?
C2 C1 H1B 108.8 . . ?
P1 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
C8 C2 C3 117.7(3) . . ?
C8 C2 C1 121.2(3) . . ?
C3 C2 C1 121.2(3) . . ?
C4 C3 C2 120.6(3) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C5 C4 C3 121.7(3) . . ?
C5 C4 H4 119.2 . . ?
C3 C4 H4 119.2 . . ?
C4 C5 C7 117.8(3) . . ?
C4 C5 C6 121.0(3) . . ?
C7 C5 C6 121.3(3) . . ?
C5 C6 P2 115.2(2) . . ?
C5 C6 H6A 108.5 . . ?
P2 C6 H6A 108.5 . . ?
C5 C6 H6B 108.5 . . ?
P2 C6 H6B 108.5 . . ?
H6A C6 H6B 107.5 . . ?
C8 C7 C5 120.8(3) . . ?
C8 C7 H7 119.6 . . ?
C5 C7 H7 119.6 . . ?
C7 C8 C2 121.4(3) . . ?
C7 C8 H8 119.3 . . ?
C2 C8 H8 119.3 . . ?
C10 C9 P3 114.63(19) . . ?
C10 C9 H9A 108.6 . . ?
P3 C9 H9A 108.6 . . ?
C10 C9 H9B 108.6 . . ?
P3 C9 H9B 108.6 . . ?
H9A C9 H9B 107.6 . . ?
C12 C10 C11 117.2(2) . . ?
C12 C10 C9 122.4(2) . . ?
C11 C10 C9 120.4(3) . . ?
C10 C11 C12 121.8(3) . 2_566 ?
C10 C11 H11 119.1 . . ?
C12 C11 H11 119.1 2_566 . ?
C10 C12 C11 121.0(3) . 2_566 ?
C10 C12 H12 119.5 . . ?
C11 C12 H12 119.5 2_566 . ?
P1 O1 Dy1 139.95(11) . . ?
P1 O2 H2A 110.6 . . ?
P1 O3 Dy1 143.07(11) . 2_675 ?
P2 O4 H4A 119.6 . . ?
P2 O5 Dy1 157.81(12) . 1_546 ?
P2 O6 Dy1 131.15(10) . 2_576 ?
P3 O7 Dy1 139.66(11) . . ?
P3 O8 H8A 113.0 . . ?
P3 O9 Dy1 144.42(12) . 2_575 ?

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
O1 P1 C1 C2 66.9(2) . . . . ?
O3 P1 C1 C2 -62.0(2) . . . . ?
O2 P1 C1 C2 -177.3(2) . . . . ?
P1 C1 C2 C8 -84.3(3) . . . . ?
P1 C1 C2 C3 95.9(3) . . . . ?
C8 C2 C3 C4 -0.9(4) . . . . ?
C1 C2 C3 C4 178.9(3) . . . . ?
C2 C3 C4 C5 -0.2(5) . . . . ?
C3 C4 C5 C7 0.3(4) . . . . ?
C3 C4 C5 C6 -179.6(3) . . . . ?
C4 C5 C6 P2 100.9(3) . . . . ?
C7 C5 C6 P2 -79.0(3) . . . . ?
O5 P2 C6 C5 -175.9(2) . . . . ?
O6 P2 C6 C5 60.1(3) . . . . ?
O4 P2 C6 C5 -59.0(3) . . . . ?
C4 C5 C7 C8 0.8(4) . . . . ?
C6 C5 C7 C8 -179.3(3) . . . . ?
C5 C7 C8 C2 -2.0(5) . . . . ?
C3 C2 C8 C7 2.0(4) . . . . ?
C1 C2 C8 C7 -177.8(3) . . . . ?
O9 P3 C9 C10 -61.4(2) . . . . ?
O7 P3 C9 C10 172.7(2) . . . . ?
O8 P3 C9 C10 56.7(2) . . . . ?
P3 C9 C10 C12 95.4(3) . . . . ?
P3 C9 C10 C11 -85.6(3) . . . . ?
C12 C10 C11 C12 -0.1(5) . . . 2_566 ?
C9 C10 C11 C12 -179.1(3) . . . 2_566 ?
C11 C10 C12 C11 0.1(5) . . . 2_566 ?
C9 C10 C12 C11 179.0(3) . . . 2_566 ?
O3 P1 O1 Dy1 -60.9(2) . . . . ?
O2 P1 O1 Dy1 61.0(2) . . . . ?
C1 P1 O1 Dy1 172.70(18) . . . . ?
O5 Dy1 O1 P1 -79.0(2) 1_564 . . . ?
O3 Dy1 O1 P1 15.2(2) 2_675 . . . ?
O9 Dy1 O1 P1 83.7(6) 2_575 . . . ?
O7 Dy1 O1 P1 98.2(2) . . . . ?
O6 Dy1 O1 P1 -177.70(19) 2_576 . . . ?
O1 P1 O3 Dy1 121.52(19) . . . 2_675 ?
O2 P1 O3 Dy1 -1.2(2) . . . 2_675 ?
C1 P1 O3 Dy1 -113.4(2) . . . 2_675 ?
O6 P2 O5 Dy1 136.3(3) . . . 1_546 ?
O4 P2 O5 Dy1 -99.1(4) . . . 1_546 ?
C6 P2 O5 Dy1 12.9(4) . . . 1_546 ?
O5 P2 O6 Dy1 4.49(19) . . . 2_576 ?
O4 P2 O6 Dy1 -119.81(15) . . . 2_576 ?
C6 P2 O6 Dy1 125.93(16) . . . 2_576 ?
O9 P3 O7 Dy1 120.56(17) . . . . ?
O8 P3 O7 Dy1 -3.0(2) . . . . ?
C9 P3 O7 Dy1 -116.78(18) . . . . ?
O5 Dy1 O7 P3 135.2(9) 1_564 . . . ?
O1 Dy1 O7 P3 89.51(18) . . . . ?
O3 Dy1 O7 P3 179.23(18) 2_675 . . . ?
O9 Dy1 O7 P3 -92.06(18) 2_575 . . . ?
O6 Dy1 O7 P3 -4.47(17) 2_576 . . . ?
O7 P3 O9 Dy1 -51.7(3) . . . 2_575 ?
O8 P3 O9 Dy1 70.9(2) . . . 2_575 ?
C9 P3 O9 Dy1 -174.2(2) . . . 2_575 ?

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
O2 H2A O7 0.78 1.87 2.646(3) 175.1 2_675
O4 H4A O2 0.77 1.95 2.710(3) 170.8 2_676
O8 H8A O6 0.90 1.80 2.695(3) 171.7 2_576

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        28.47
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.107
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2031257'
_audit_update_record             
;
2020-09-10 deposited with the CCDC.	2020-12-14 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H15 Ho O9 P3'
_chemical_formula_sum            'C12 H15 Ho O9 P3'
_chemical_formula_weight         561.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.0404(3)
_cell_length_b                   9.4303(3)
_cell_length_c                   12.0760(4)
_cell_angle_alpha                67.7680(10)
_cell_angle_beta                 70.814(2)
_cell_angle_gamma                64.9800(10)
_cell_volume                     845.93(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9928
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      28.33

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             542
_exptl_absorpt_coefficient_mu    5.005
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4343
_exptl_absorpt_correction_T_max  0.6902
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15312
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.48
_diffrn_reflns_theta_max         28.33
_reflns_number_total             4177
_reflns_number_gt                3991
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0238P)²+0.1238P] where P=(Fo²+2Fc²)/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         4177
_refine_ls_number_parameters     226
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0187
_refine_ls_R_factor_gt           0.0174
_refine_ls_wR_factor_ref         0.0407
_refine_ls_wR_factor_gt          0.0400
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.001
_refine_ls_shift/su_max          0.005
_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
Ho1 Ho 0.162829(11) 1.197180(10) 0.005998(7) 0.01147(4) Uani 1 1 d . . .
P1 P 0.49434(7) 1.06605(6) 0.15272(5) 0.01354(11) Uani 1 1 d . . .
P2 P 0.22721(7) 0.58395(6) 0.84581(5) 0.01445(11) Uani 1 1 d . . .
P3 P 0.05520(7) 0.83392(6) 0.17689(5) 0.01267(11) Uani 1 1 d . . .
C1 C 0.5038(3) 1.0562(3) 0.30166(19) 0.0167(4) Uani 1 1 d . . .
H1A H 0.6203 1.0346 0.3031 0.020 Uiso 1 1 calc R . .
H1B H 0.4351 1.1634 0.3174 0.020 Uiso 1 1 calc R . .
C2 C 0.4438(3) 0.9265(3) 0.40242(19) 0.0169(4) Uani 1 1 d . . .
C3 C 0.5555(3) 0.7740(3) 0.44780(19) 0.0194(5) Uani 1 1 d . . .
H3 H 0.6714 0.7501 0.4143 0.023 Uiso 1 1 calc R . .
C4 C 0.4987(3) 0.6560(3) 0.54202(19) 0.0201(5) Uani 1 1 d . . .
H4 H 0.5767 0.5519 0.5715 0.024 Uiso 1 1 calc R . .
C5 C 0.3308(3) 0.6873(3) 0.59361(19) 0.0181(4) Uani 1 1 d . . .
C6 C 0.2718(3) 0.5585(3) 0.69705(19) 0.0198(5) Uani 1 1 d . . .
H6A H 0.3584 0.4505 0.6957 0.024 Uiso 1 1 calc R . .
H6B H 0.1700 0.5587 0.6828 0.024 Uiso 1 1 calc R . .
C7 C 0.2189(3) 0.8406(3) 0.5481(2) 0.0204(5) Uani 1 1 d . . .
H7 H 0.1032 0.8651 0.5824 0.024 Uiso 1 1 calc R . .
C8 C 0.2750(3) 0.9579(3) 0.4533(2) 0.0207(5) Uani 1 1 d . . .
H8 H 0.1968 1.0612 0.4227 0.025 Uiso 1 1 calc R . .
C9 C 0.1827(3) 0.6785(3) 0.28361(19) 0.0174(4) Uani 1 1 d . . .
H9A H 0.2739 0.6005 0.2410 0.021 Uiso 1 1 calc R . .
H9B H 0.2341 0.7302 0.3112 0.021 Uiso 1 1 calc R . .
C10 C 0.0878(3) 0.5853(3) 0.39452(19) 0.0167(4) Uani 1 1 d . . .
C11 C 0.0015(3) 0.6472(3) 0.4941(2) 0.0232(5) Uani 1 1 d . . .
H11 H 0.0010 0.7495 0.4912 0.028 Uiso 1 1 calc R . .
C12 C 0.0844(3) 0.4368(3) 0.4020(2) 0.0227(5) Uani 1 1 d . . .
H12 H 0.1415 0.3915 0.3351 0.027 Uiso 1 1 calc R . .
O1 O 0.31503(19) 1.12139(18) 0.14504(13) 0.0181(3) Uani 1 1 d . . .
O2 O 0.57035(19) 1.20504(17) 0.06465(13) 0.0198(3) Uani 1 1 d . . .
H2A H 0.6513 1.1697 0.0200 0.030 Uiso 1 1 d R . .
O3 O 0.60636(18) 0.90920(17) 0.12032(13) 0.0169(3) Uani 1 1 d . . .
O4 O 0.39640(19) 0.58211(19) 0.85553(15) 0.0233(4) Uani 1 1 d . . .
H4A H 0.3976 0.6506 0.8745 0.035 Uiso 1 1 d R . .
O5 O 0.1846(2) 0.43980(18) 0.93805(13) 0.0186(3) Uani 1 1 d . . .
O6 O 0.08862(19) 0.74535(17) 0.85612(13) 0.0186(3) Uani 1 1 d . . .
O7 O 0.15825(18) 0.93309(16) 0.07864(13) 0.0152(3) Uani 1 1 d . . .
O8 O -0.08812(19) 0.94857(18) 0.25266(14) 0.0217(3) Uani 1 1 d . . .
H8A H -0.0901 1.0515 0.2241 0.033 Uiso 1 1 d R . .
O9 O -0.0162(2) 0.75549(18) 0.13030(14) 0.0189(3) Uani 1 1 d . . .


_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
Ho1 O5 2.1911(14) 1_564 ?
Ho1 O3 2.2321(14) 2_675 ?
Ho1 O1 2.2365(15) . ?
Ho1 O9 2.2457(16) 2_575 ?
Ho1 O7 2.3203(13) . ?
Ho1 O6 2.3209(14) 2_576 ?
P1 O1 1.5018(16) . ?
P1 O3 1.5091(15) . ?
P1 O2 1.5962(15) . ?
P1 C1 1.794(2) . ?
P2 O5 1.5007(15) . ?
P2 O6 1.5264(15) . ?
P2 O4 1.5645(17) . ?
P2 C6 1.793(2) . ?
P3 O9 1.4959(17) . ?
P3 O7 1.5235(14) . ?
P3 O8 1.5715(16) . ?
P3 C9 1.804(2) . ?
C1 C2 1.507(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.388(3) . ?
C2 C8 1.390(3) . ?
C3 C4 1.392(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.385(3) . ?
C4 H4 0.9500 . ?
C5 C7 1.393(3) . ?
C5 C6 1.511(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.387(3) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.515(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C12 1.382(3) . ?
C10 C11 1.387(3) . ?
C11 C12 1.390(3) 2_566 ?
C11 H11 0.9500 . ?
C12 C11 1.390(3) 2_566 ?
C12 H12 0.9500 . ?
O2 H2A 0.7795 . ?
O3 Ho1 2.2321(14) 2_675 ?
O4 H4A 0.7678 . ?
O5 Ho1 2.1911(14) 1_546 ?
O6 Ho1 2.3209(14) 2_576 ?
O8 H8A 0.8934 . ?
O9 Ho1 2.2457(16) 2_575 ?

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
O5 Ho1 O3 94.31(5) 1_564 2_675 ?
O5 Ho1 O1 90.67(6) 1_564 . ?
O3 Ho1 O1 89.43(6) 2_675 . ?
O5 Ho1 O9 95.21(6) 1_564 2_575 ?
O3 Ho1 O9 88.22(6) 2_675 2_575 ?
O1 Ho1 O9 173.81(5) . 2_575 ?
O5 Ho1 O7 176.22(5) 1_564 . ?
O3 Ho1 O7 83.12(5) 2_675 . ?
O1 Ho1 O7 86.54(5) . . ?
O9 Ho1 O7 87.50(5) 2_575 . ?
O5 Ho1 O6 98.30(5) 1_564 2_576 ?
O3 Ho1 O6 166.99(5) 2_675 2_576 ?
O1 Ho1 O6 93.58(5) . 2_576 ?
O9 Ho1 O6 87.47(6) 2_575 2_576 ?
O7 Ho1 O6 84.43(5) . 2_576 ?
O1 P1 O3 115.82(9) . . ?
O1 P1 O2 109.20(9) . . ?
O3 P1 O2 107.80(8) . . ?
O1 P1 C1 108.92(10) . . ?
O3 P1 C1 111.19(10) . . ?
O2 P1 C1 103.13(9) . . ?
O5 P2 O6 112.38(9) . . ?
O5 P2 O4 110.81(9) . . ?
O6 P2 O4 110.94(9) . . ?
O5 P2 C6 107.85(10) . . ?
O6 P2 C6 111.37(10) . . ?
O4 P2 C6 103.07(10) . . ?
O9 P3 O7 114.91(9) . . ?
O9 P3 O8 110.13(9) . . ?
O7 P3 O8 108.11(8) . . ?
O9 P3 C9 109.04(10) . . ?
O7 P3 C9 108.85(9) . . ?
O8 P3 C9 105.36(10) . . ?
C2 C1 P1 113.36(16) . . ?
C2 C1 H1A 108.9 . . ?
P1 C1 H1A 108.9 . . ?
C2 C1 H1B 108.9 . . ?
P1 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
C3 C2 C8 118.4(2) . . ?
C3 C2 C1 120.9(2) . . ?
C8 C2 C1 120.6(2) . . ?
C2 C3 C4 120.4(2) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C5 C4 C3 121.3(2) . . ?
C5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
C4 C5 C7 118.2(2) . . ?
C4 C5 C6 120.5(2) . . ?
C7 C5 C6 121.3(2) . . ?
C5 C6 P2 114.61(16) . . ?
C5 C6 H6A 108.6 . . ?
P2 C6 H6A 108.6 . . ?
C5 C6 H6B 108.6 . . ?
P2 C6 H6B 108.6 . . ?
H6A C6 H6B 107.6 . . ?
C8 C7 C5 120.6(2) . . ?
C8 C7 H7 119.7 . . ?
C5 C7 H7 119.7 . . ?
C7 C8 C2 121.0(2) . . ?
C7 C8 H8 119.5 . . ?
C2 C8 H8 119.5 . . ?
C10 C9 P3 113.77(15) . . ?
C10 C9 H9A 108.8 . . ?
P3 C9 H9A 108.8 . . ?
C10 C9 H9B 108.8 . . ?
P3 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
C12 C10 C11 117.42(19) . . ?
C12 C10 C9 122.3(2) . . ?
C11 C10 C9 120.2(2) . . ?
C10 C11 C12 121.6(2) . 2_566 ?
C10 C11 H11 119.2 . . ?
C12 C11 H11 119.2 2_566 . ?
C10 C12 C11 121.0(2) . 2_566 ?
C10 C12 H12 119.5 . . ?
C11 C12 H12 119.5 2_566 . ?
P1 O1 Ho1 139.28(9) . . ?
P1 O2 H2A 110.5 . . ?
P1 O3 Ho1 142.86(9) . 2_675 ?
P2 O4 H4A 119.5 . . ?
P2 O5 Ho1 156.86(10) . 1_546 ?
P2 O6 Ho1 131.25(8) . 2_576 ?
P3 O7 Ho1 139.62(9) . . ?
P3 O8 H8A 113.2 . . ?
P3 O9 Ho1 143.61(9) . 2_575 ?

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
O1 P1 C1 C2 66.32(18) . . . . ?
O3 P1 C1 C2 -62.49(18) . . . . ?
O2 P1 C1 C2 -177.77(16) . . . . ?
P1 C1 C2 C3 96.5(2) . . . . ?
P1 C1 C2 C8 -84.4(2) . . . . ?
C8 C2 C3 C4 0.0(3) . . . . ?
C1 C2 C3 C4 179.1(2) . . . . ?
C2 C3 C4 C5 -0.6(4) . . . . ?
C3 C4 C5 C7 0.4(3) . . . . ?
C3 C4 C5 C6 -179.1(2) . . . . ?
C4 C5 C6 P2 100.4(2) . . . . ?
C7 C5 C6 P2 -79.0(3) . . . . ?
O5 P2 C6 C5 -175.34(16) . . . . ?
O6 P2 C6 C5 60.91(19) . . . . ?
O4 P2 C6 C5 -58.09(19) . . . . ?
C4 C5 C7 C8 0.4(4) . . . . ?
C6 C5 C7 C8 179.8(2) . . . . ?
C5 C7 C8 C2 -0.9(4) . . . . ?
C3 C2 C8 C7 0.7(3) . . . . ?
C1 C2 C8 C7 -178.4(2) . . . . ?
O9 P3 C9 C10 -61.23(19) . . . . ?
O7 P3 C9 C10 172.71(15) . . . . ?
O8 P3 C9 C10 56.96(18) . . . . ?
P3 C9 C10 C12 96.5(2) . . . . ?
P3 C9 C10 C11 -84.1(2) . . . . ?
C12 C10 C11 C12 0.5(4) . . . 2_566 ?
C9 C10 C11 C12 -178.9(2) . . . 2_566 ?
C11 C10 C12 C11 -0.5(4) . . . 2_566 ?
C9 C10 C12 C11 178.9(2) . . . 2_566 ?
O3 P1 O1 Ho1 -61.69(16) . . . . ?
O2 P1 O1 Ho1 60.19(16) . . . . ?
C1 P1 O1 Ho1 172.13(13) . . . . ?
O5 Ho1 O1 P1 -78.87(14) 1_564 . . . ?
O3 Ho1 O1 P1 15.43(14) 2_675 . . . ?
O7 Ho1 O1 P1 98.58(14) . . . . ?
O6 Ho1 O1 P1 -177.23(14) 2_576 . . . ?
O1 P1 O3 Ho1 122.13(15) . . . 2_675 ?
O2 P1 O3 Ho1 -0.49(19) . . . 2_675 ?
C1 P1 O3 Ho1 -112.84(16) . . . 2_675 ?
O6 P2 O5 Ho1 134.9(2) . . . 1_546 ?
O4 P2 O5 Ho1 -100.3(3) . . . 1_546 ?
C6 P2 O5 Ho1 11.8(3) . . . 1_546 ?
O5 P2 O6 Ho1 3.87(16) . . . 2_576 ?
O4 P2 O6 Ho1 -120.80(12) . . . 2_576 ?
C6 P2 O6 Ho1 125.01(12) . . . 2_576 ?
O9 P3 O7 Ho1 121.34(13) . . . . ?
O8 P3 O7 Ho1 -2.10(17) . . . . ?
C9 P3 O7 Ho1 -116.07(14) . . . . ?
O3 Ho1 O7 P3 178.11(15) 2_675 . . . ?
O1 Ho1 O7 P3 88.27(14) . . . . ?
O9 Ho1 O7 P3 -93.38(14) 2_575 . . . ?
O6 Ho1 O7 P3 -5.68(14) 2_576 . . . ?
O7 P3 O9 Ho1 -50.26(19) . . . 2_575 ?
O8 P3 O9 Ho1 72.10(17) . . . 2_575 ?
C9 P3 O9 Ho1 -172.75(15) . . . 2_575 ?

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
O2 H2A O7 0.78 1.85 2.631(2) 174.8 2_675
O4 H4A O2 0.77 1.93 2.686(2) 170.5 2_676
O8 H8A O6 0.89 1.79 2.680(2) 171.1 2_576

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        28.33
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.790
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.099
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2031256'
_audit_update_record             
;
2020-09-10 deposited with the CCDC.	2020-12-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H15 O9 P3 Tb'
_chemical_formula_sum            'C12 H15 O9 P3 Tb'
_chemical_formula_weight         555.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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           Triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.0909(5)
_cell_length_b                   9.4752(4)
_cell_length_c                   12.1186(6)
_cell_angle_alpha                67.655(2)
_cell_angle_beta                 70.568(3)
_cell_angle_gamma                64.578(2)
_cell_volume                     853.87(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5624
_cell_measurement_theta_min      2.98
_cell_measurement_theta_max      30.24

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             538
_exptl_absorpt_coefficient_mu    4.467
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6162
_exptl_absorpt_correction_T_max  0.7164
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19233
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_sigmaI/netI    0.0577
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.48
_diffrn_reflns_theta_max         30.69
_reflns_number_total             5219
_reflns_number_gt                4577
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0221P)²+0.0000P] where P=(Fo²+2Fc²)/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         5219
_refine_ls_number_parameters     226
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0322
_refine_ls_wR_factor_ref         0.0659
_refine_ls_wR_factor_gt          0.0628
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.000
_refine_ls_shift/su_max          0.003
_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
Tb1 Tb 0.161660(19) 1.198502(17) 0.006055(13) 0.01677(5) Uani 1 1 d . . .
P1 P 0.49435(11) 1.06779(10) 0.15291(7) 0.01898(17) Uani 1 1 d . . .
P2 P 0.22902(11) 0.58497(10) 0.84383(8) 0.02014(18) Uani 1 1 d . . .
P3 P 0.05592(11) 0.83337(10) 0.17736(7) 0.01761(17) Uani 1 1 d . . .
C1 C 0.5019(5) 1.0571(4) 0.3013(3) 0.0260(7) Uani 1 1 d . . .
H1A H 0.6179 1.0357 0.3029 0.031 Uiso 1 1 calc R . .
H1B H 0.4326 1.1641 0.3171 0.031 Uiso 1 1 calc R . .
C2 C 0.4433(4) 0.9286(4) 0.4017(3) 0.0224(7) Uani 1 1 d . . .
C3 C 0.5560(5) 0.7758(5) 0.4471(3) 0.0299(8) Uani 1 1 d . . .
H3 H 0.6716 0.7517 0.4135 0.036 Uiso 1 1 calc R . .
C4 C 0.5004(5) 0.6599(5) 0.5402(3) 0.0309(8) Uani 1 1 d . . .
H4 H 0.5792 0.5565 0.5695 0.037 Uiso 1 1 calc R . .
C5 C 0.3332(5) 0.6887(4) 0.5927(3) 0.0269(8) Uani 1 1 d . . .
C6 C 0.2755(5) 0.5609(4) 0.6955(3) 0.0297(8) Uani 1 1 d . . .
H6A H 0.3627 0.4533 0.6940 0.036 Uiso 1 1 calc R . .
H6B H 0.1746 0.5609 0.6809 0.036 Uiso 1 1 calc R . .
C7 C 0.2212(5) 0.8420(4) 0.5473(3) 0.0303(8) Uani 1 1 d . . .
H7 H 0.1058 0.8668 0.5820 0.036 Uiso 1 1 calc R . .
C8 C 0.2760(5) 0.9581(4) 0.4525(3) 0.0302(8) Uani 1 1 d . . .
H8 H 0.1970 1.0605 0.4215 0.036 Uiso 1 1 calc R . .
C9 C 0.1814(4) 0.6772(4) 0.2842(3) 0.0246(7) Uani 1 1 d . . .
H9A H 0.2724 0.5989 0.2418 0.029 Uiso 1 1 calc R . .
H9B H 0.2329 0.7279 0.3118 0.029 Uiso 1 1 calc R . .
C10 C 0.0869(4) 0.5851(4) 0.3948(3) 0.0218(7) Uani 1 1 d . . .
C11 C 0.0042(5) 0.6434(5) 0.4956(3) 0.0333(9) Uani 1 1 d . . .
H11 H 0.0061 0.7437 0.4939 0.040 Uiso 1 1 calc R . .
C12 C 0.0811(5) 0.4391(4) 0.4011(3) 0.0332(9) Uani 1 1 d . . .
H12 H 0.1364 0.3947 0.3338 0.040 Uiso 1 1 calc R . .
O1 O 0.3161(3) 1.1241(3) 0.1441(2) 0.0265(5) Uani 1 1 d . . .
O2 O 0.5703(3) 1.2052(3) 0.0659(2) 0.0299(6) Uani 1 1 d . . .
H2A H 0.6512 1.1699 0.0213 0.045 Uiso 1 1 d R . .
O3 O 0.6065(3) 0.9113(3) 0.1207(2) 0.0251(5) Uani 1 1 d . . .
O4 O 0.3963(3) 0.5803(3) 0.8564(2) 0.0334(6) Uani 1 1 d . . .
H4A H 0.3975 0.6488 0.8754 0.050 Uiso 1 1 d R . .
O5 O 0.1849(3) 0.4421(3) 0.9350(2) 0.0298(6) Uani 1 1 d . . .
O6 O 0.0918(3) 0.7465(3) 0.8537(2) 0.0266(5) Uani 1 1 d . . .
O7 O 0.1592(3) 0.9315(3) 0.08073(19) 0.0219(5) Uani 1 1 d . . .
O8 O -0.0880(3) 0.9467(3) 0.2528(2) 0.0336(6) Uani 1 1 d . . .
H8A H -0.0900 1.0497 0.2242 0.050 Uiso 1 1 d R . .
O9 O -0.0135(3) 0.7564(3) 0.1294(2) 0.0294(6) Uani 1 1 d . . .


_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
Tb1 O5 2.213(2) 1_564 ?
Tb1 O3 2.250(2) 2_675 ?
Tb1 O1 2.255(2) . ?
Tb1 O9 2.266(2) 2_575 ?
Tb1 O6 2.347(2) 2_576 ?
Tb1 O7 2.349(2) . ?
P1 O1 1.501(3) . ?
P1 O3 1.506(2) . ?
P1 O2 1.590(2) . ?
P1 C1 1.785(3) . ?
P2 O5 1.499(2) . ?
P2 O6 1.521(2) . ?
P2 O4 1.559(3) . ?
P2 C6 1.785(3) . ?
P3 O9 1.493(3) . ?
P3 O7 1.519(2) . ?
P3 O8 1.564(3) . ?
P3 C9 1.801(3) . ?
C1 C2 1.499(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C8 1.383(5) . ?
C2 C3 1.395(5) . ?
C3 C4 1.374(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(5) . ?
C4 H4 0.9500 . ?
C5 C7 1.394(5) . ?
C5 C6 1.502(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.381(5) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.511(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C12 1.379(5) . ?
C10 C11 1.381(5) . ?
C11 C12 1.382(5) 2_566 ?
C11 H11 0.9500 . ?
C12 C11 1.382(5) 2_566 ?
C12 H12 0.9500 . ?
O2 H2A 0.7795 . ?
O3 Tb1 2.250(2) 2_675 ?
O4 H4A 0.7717 . ?
O5 Tb1 2.213(2) 1_546 ?
O6 Tb1 2.347(2) 2_576 ?
O8 H8A 0.8968 . ?
O9 Tb1 2.266(2) 2_575 ?

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
O5 Tb1 O3 94.13(9) 1_564 2_675 ?
O5 Tb1 O1 90.36(9) 1_564 . ?
O3 Tb1 O1 89.28(9) 2_675 . ?
O5 Tb1 O9 95.60(9) 1_564 2_575 ?
O3 Tb1 O9 88.16(9) 2_675 2_575 ?
O1 Tb1 O9 173.67(8) . 2_575 ?
O5 Tb1 O6 99.80(9) 1_564 2_576 ?
O3 Tb1 O6 165.68(8) 2_675 2_576 ?
O1 Tb1 O6 93.90(9) . 2_576 ?
O9 Tb1 O6 87.20(9) 2_575 2_576 ?
O5 Tb1 O7 175.60(9) 1_564 . ?
O3 Tb1 O7 82.59(8) 2_675 . ?
O1 Tb1 O7 86.69(8) . . ?
O9 Tb1 O7 87.24(8) 2_575 . ?
O6 Tb1 O7 83.66(8) 2_576 . ?
O1 P1 O3 115.74(15) . . ?
O1 P1 O2 109.14(14) . . ?
O3 P1 O2 107.79(13) . . ?
O1 P1 C1 109.05(16) . . ?
O3 P1 C1 111.10(16) . . ?
O2 P1 C1 103.28(15) . . ?
O5 P2 O6 112.48(14) . . ?
O5 P2 O4 110.47(15) . . ?
O6 P2 O4 110.74(14) . . ?
O5 P2 C6 108.01(16) . . ?
O6 P2 C6 111.25(16) . . ?
O4 P2 C6 103.49(17) . . ?
O9 P3 O7 114.82(14) . . ?
O9 P3 O8 110.00(16) . . ?
O7 P3 O8 108.40(13) . . ?
O9 P3 C9 109.00(16) . . ?
O7 P3 C9 108.89(15) . . ?
O8 P3 C9 105.30(15) . . ?
C2 C1 P1 114.1(2) . . ?
C2 C1 H1A 108.7 . . ?
P1 C1 H1A 108.7 . . ?
C2 C1 H1B 108.7 . . ?
P1 C1 H1B 108.7 . . ?
H1A C1 H1B 107.6 . . ?
C8 C2 C3 118.0(3) . . ?
C8 C2 C1 121.1(3) . . ?
C3 C2 C1 120.9(3) . . ?
C4 C3 C2 120.2(3) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 122.3(3) . . ?
C3 C4 H4 118.9 . . ?
C5 C4 H4 118.9 . . ?
C4 C5 C7 117.2(3) . . ?
C4 C5 C6 121.4(3) . . ?
C7 C5 C6 121.4(3) . . ?
C5 C6 P2 115.3(3) . . ?
C5 C6 H6A 108.5 . . ?
P2 C6 H6A 108.5 . . ?
C5 C6 H6B 108.5 . . ?
P2 C6 H6B 108.5 . . ?
H6A C6 H6B 107.5 . . ?
C8 C7 C5 120.8(3) . . ?
C8 C7 H7 119.6 . . ?
C5 C7 H7 119.6 . . ?
C7 C8 C2 121.5(3) . . ?
C7 C8 H8 119.3 . . ?
C2 C8 H8 119.3 . . ?
C10 C9 P3 114.3(2) . . ?
C10 C9 H9A 108.7 . . ?
P3 C9 H9A 108.7 . . ?
C10 C9 H9B 108.7 . . ?
P3 C9 H9B 108.7 . . ?
H9A C9 H9B 107.6 . . ?
C12 C10 C11 117.0(3) . . ?
C12 C10 C9 122.2(3) . . ?
C11 C10 C9 120.8(3) . . ?
C10 C11 C12 122.3(3) . 2_566 ?
C10 C11 H11 118.8 . . ?
C12 C11 H11 118.8 2_566 . ?
C10 C12 C11 120.7(3) . 2_566 ?
C10 C12 H12 119.6 . . ?
C11 C12 H12 119.6 2_566 . ?
P1 O1 Tb1 140.25(14) . . ?
P1 O2 H2A 110.7 . . ?
P1 O3 Tb1 143.40(14) . 2_675 ?
P2 O4 H4A 119.7 . . ?
P2 O5 Tb1 157.96(16) . 1_546 ?
P2 O6 Tb1 130.04(13) . 2_576 ?
P3 O7 Tb1 139.79(13) . . ?
P3 O8 H8A 112.7 . . ?
P3 O9 Tb1 144.80(15) . 2_575 ?

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
O1 P1 C1 C2 66.7(3) . . . . ?
O3 P1 C1 C2 -62.1(3) . . . . ?
O2 P1 C1 C2 -177.4(3) . . . . ?
P1 C1 C2 C8 -84.0(4) . . . . ?
P1 C1 C2 C3 96.2(4) . . . . ?
C8 C2 C3 C4 -0.5(5) . . . . ?
C1 C2 C3 C4 179.3(3) . . . . ?
C2 C3 C4 C5 -0.2(6) . . . . ?
C3 C4 C5 C7 -0.1(6) . . . . ?
C3 C4 C5 C6 -179.2(3) . . . . ?
C4 C5 C6 P2 100.3(4) . . . . ?
C7 C5 C6 P2 -78.7(4) . . . . ?
O5 P2 C6 C5 -176.3(3) . . . . ?
O6 P2 C6 C5 59.8(3) . . . . ?
O4 P2 C6 C5 -59.1(3) . . . . ?
C4 C5 C7 C8 1.1(6) . . . . ?
C6 C5 C7 C8 -179.8(3) . . . . ?
C5 C7 C8 C2 -1.9(6) . . . . ?
C3 C2 C8 C7 1.6(5) . . . . ?
C1 C2 C8 C7 -178.2(3) . . . . ?
O9 P3 C9 C10 -62.0(3) . . . . ?
O7 P3 C9 C10 172.1(2) . . . . ?
O8 P3 C9 C10 56.0(3) . . . . ?
P3 C9 C10 C12 95.3(4) . . . . ?
P3 C9 C10 C11 -85.7(4) . . . . ?
C12 C10 C11 C12 0.0(7) . . . 2_566 ?
C9 C10 C11 C12 -179.0(4) . . . 2_566 ?
C11 C10 C12 C11 0.0(6) . . . 2_566 ?
C9 C10 C12 C11 179.0(4) . . . 2_566 ?
O3 P1 O1 Tb1 -60.4(3) . . . . ?
O2 P1 O1 Tb1 61.4(3) . . . . ?
C1 P1 O1 Tb1 173.5(2) . . . . ?
O5 Tb1 O1 P1 -79.1(2) 1_564 . . . ?
O3 Tb1 O1 P1 15.1(2) 2_675 . . . ?
O6 Tb1 O1 P1 -178.9(2) 2_576 . . . ?
O7 Tb1 O1 P1 97.7(2) . . . . ?
O1 P1 O3 Tb1 121.2(2) . . . 2_675 ?
O2 P1 O3 Tb1 -1.2(3) . . . 2_675 ?
C1 P1 O3 Tb1 -113.7(3) . . . 2_675 ?
O6 P2 O5 Tb1 136.4(4) . . . 1_546 ?
O4 P2 O5 Tb1 -99.3(5) . . . 1_546 ?
C6 P2 O5 Tb1 13.3(5) . . . 1_546 ?
O5 P2 O6 Tb1 4.2(2) . . . 2_576 ?
O4 P2 O6 Tb1 -119.96(19) . . . 2_576 ?
C6 P2 O6 Tb1 125.5(2) . . . 2_576 ?
O9 P3 O7 Tb1 119.9(2) . . . . ?
O8 P3 O7 Tb1 -3.5(3) . . . . ?
C9 P3 O7 Tb1 -117.6(2) . . . . ?
O3 Tb1 O7 P3 180.0(2) 2_675 . . . ?
O1 Tb1 O7 P3 90.3(2) . . . . ?
O9 Tb1 O7 P3 -91.5(2) 2_575 . . . ?
O6 Tb1 O7 P3 -4.0(2) 2_576 . . . ?
O7 P3 O9 Tb1 -51.9(3) . . . 2_575 ?
O8 P3 O9 Tb1 70.7(3) . . . 2_575 ?
C9 P3 O9 Tb1 -174.3(3) . . . 2_575 ?

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
O2 H2A O7 0.78 1.87 2.644(3) 175.0 2_675
O4 H4A O2 0.77 1.93 2.699(3) 171.0 2_676
O8 H8A O6 0.90 1.79 2.684(3) 171.9 2_576

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        30.69
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.157
