# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1400186'
_audit_update_record             
;
2015-08-24 deposited with the CCDC.
2015-09-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H34 Dy2 O23 P6'
_chemical_formula_weight         1165.30

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'

_space_group_crystal_system      cubic
_space_group_IT_number           199
_space_group_name_H-M_alt        'I 21 3'
_space_group_name_Hall           'I 2b 2c 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   15.9547(8)
_cell_length_b                   15.9547(8)
_cell_length_c                   15.9547(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4061.3(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      3.128
_cell_measurement_theta_max      26.310

_exptl_crystal_description       cubic
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.906
_exptl_crystal_F_000             2264
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_exptl_absorpt_coefficient_mu    3.966
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.418
_exptl_absorpt_correction_T_max  0.435
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4423
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.128
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.001
_diffrn_measured_fraction_theta_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 1.001
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 1.003
_diffrn_reflns_point_group_measured_fraction_full 0.969
_reflns_number_total             1204
_reflns_number_gt                1112
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.792
_reflns_Friedel_fraction_max     1.006
_reflns_Friedel_fraction_full    0.969

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_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.
;
_vrf_PLAT417_4                   
;
PROBLEM: Short Inter D-H..H-D H1B .. H3W .. 1.75 Ang.
RESPONSE: O2W is situated at a special position.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0200P)²+0.0424P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 472 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.023(14)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         1204
_refine_ls_number_parameters     90
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0243
_refine_ls_wR_factor_ref         0.0490
_refine_ls_wR_factor_gt          0.0473
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.066
_refine_ls_shift/su_mean         0.007

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
Dy1 Dy 1.14114(2) 1.14114(2) 0.14114(2) 0.01432(2) Uani 1 3 d S T P . .
O1 O 1.04831(9) 0.89362(10) 0.11340(10) 0.0396(5) Uani 1 1 d . . . . .
H1B H 1.0337 0.8495 0.1353 0.059 Uiso 1 1 calc R U . . .
O2 O 1.15759(9) 1.00307(8) 0.12465(9) 0.0295(5) Uani 1 1 d . . . . .
O3 O 1.16036(10) 0.87637(9) 0.22022(8) 0.0332(5) Uani 1 1 d . . . . .
P1 P 1.14263(3) 0.91140(3) 0.13526(3) 0.02120(13) Uani 1 1 d . . . . .
C1 C 1.2500 0.89885(18) 0.0000 0.0220(9) Uani 1 2 d S T P . .
H1A H 1.2500 0.9571 0.0000 0.026 Uiso 1 2 calc R U P . .
C2 C 1.20478(13) 0.85608(14) 0.06014(12) 0.0260(6) Uani 1 1 d . . . . .
C3 C 1.20559(18) 0.76802(15) 0.06012(17) 0.0507(8) Uani 1 1 d . . . . .
H3A H 1.1759 0.7390 0.1010 0.061 Uiso 1 1 calc R U . . .
C4 C 1.2500 0.7240(2) 0.0000 0.0673(15) Uani 1 2 d S T P . .
O1W O 0.98211(12) 0.98211(12) -0.01789(12) 0.0588(9) Uani 1 3 d S T P . .
H1W H 0.9728 1.0303 -0.0399 0.071 Uiso 0.3333 1 d R U P . .
H2W H 0.9319 0.9677 -0.0190 0.071 Uiso 0.3333 1 d R U P . .
O2W O 1.0038(5) 0.7562(4) 0.18374(19) 0.0696(11) Uani 0.5 1 d . . P A -1
H3W H 0.9741 0.7576 0.1400 0.083 Uiso 0.5 1 d R U P A -1
H4W H 1.0131 0.7269 0.2268 0.083 Uiso 0.5 1 d R U P A -1
C5 C 1.2689(5) 0.6282(2) 0.0151(5) 0.083(2) Uani 0.5 1 d . . P B -1
H5A H 1.2234 0.6034 0.0457 0.125 Uiso 0.5 1 calc R U P B -1
H5B H 1.3197 0.6225 0.0467 0.125 Uiso 0.5 1 calc R U P B -1
H5C H 1.2749 0.6004 -0.0379 0.125 Uiso 0.5 1 calc R U P B -1


_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 O2 2.2339(12) . ?
Dy1 O2 2.2340(12) 5_654 ?
Dy1 O2 2.2340(12) 9_564 ?
Dy1 O3 2.2506(13) 16_465 ?
Dy1 O3 2.2506(13) 24_663 ?
Dy1 O3 2.2506(14) 20_645 ?
O1 P1 1.5705(16) . ?
O2 P1 1.4916(13) . ?
O3 P1 1.4933(14) . ?
O3 Dy1 2.2506(13) 16_465 ?
P1 C2 1.788(2) . ?
C1 C2 1.381(2) 15_744 ?
C1 C2 1.381(2) . ?
C2 C3 1.405(3) . ?
C3 C4 1.384(3) . ?
C4 C3 1.384(3) 15_744 ?
C4 C5 1.576(5) . ?

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
O2 Dy1 O2 90.78(5) . 5_654 ?
O2 Dy1 O2 90.78(5) . 9_564 ?
O2 Dy1 O2 90.78(5) 5_654 9_564 ?
O2 Dy1 O3 88.70(5) . 16_465 ?
O2 Dy1 O3 178.86(5) 5_654 16_465 ?
O2 Dy1 O3 90.24(5) 9_564 16_465 ?
O2 Dy1 O3 178.86(5) . 24_663 ?
O2 Dy1 O3 90.24(5) 5_654 24_663 ?
O2 Dy1 O3 88.70(5) 9_564 24_663 ?
O3 Dy1 O3 90.29(5) 16_465 24_663 ?
O2 Dy1 O3 90.25(5) . 20_645 ?
O2 Dy1 O3 88.70(5) 5_654 20_645 ?
O2 Dy1 O3 178.86(5) 9_564 20_645 ?
O3 Dy1 O3 90.29(5) 16_465 20_645 ?
O3 Dy1 O3 90.29(5) 24_663 20_645 ?
P1 O2 Dy1 159.19(9) . . ?
P1 O3 Dy1 155.90(9) . 16_465 ?
O2 P1 O3 116.08(8) . . ?
O2 P1 O1 107.77(9) . . ?
O3 P1 O1 108.39(9) . . ?
O2 P1 C2 108.61(9) . . ?
O3 P1 C2 108.58(9) . . ?
O1 P1 C2 107.06(9) . . ?
C2 C1 C2 120.8(3) 15_744 . ?
C1 C2 C3 119.3(2) . . ?
C1 C2 P1 120.76(18) . . ?
C3 C2 P1 119.92(17) . . ?
C4 C3 C2 120.8(2) . . ?
C3 C4 C3 119.0(3) 15_744 . ?
C3 C4 C5 120.0(3) 15_744 . ?
C3 C4 C5 118.9(3) . . ?

_refine_diff_density_max         0.489
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.077

_shelxl_version_number           2013-2

####################################################################### 
# 
# 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 1400187'
_audit_update_record             
;
2015-08-24 deposited with the CCDC.
2015-09-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H34 Eu2 O23 P6'
_chemical_formula_weight         1144.22

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'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           199
_space_group_name_H-M_alt        'I 21 3'
_space_group_name_Hall           'I 2b 2c 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   16.0668(9)
_cell_length_b                   16.0668(9)
_cell_length_c                   16.0668(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4147.5(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.535
_cell_measurement_theta_max      27.437

_exptl_crystal_description       cubic
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_F_000             2240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    3.305
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.516
_exptl_absorpt_correction_T_max  0.521
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2970
_diffrn_reflns_av_unetI/netI     0.0656
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.535
_diffrn_reflns_theta_max         24.960
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.001
_diffrn_measured_fraction_theta_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 1.001
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.973
_reflns_number_total             1221
_reflns_number_gt                1093
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.780
_reflns_Friedel_fraction_max     0.989
_reflns_Friedel_fraction_full    0.967

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_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.
;
_vrf_PLAT417_1                   
;
PROBLEM: Short Inter D-H..H-D H1B .. H3W .. 1.62 Ang.
RESPONSE: O2W is situated at a special position (1.00 0.75 0.183996).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0262P)²]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 437 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.04(3)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         1221
_refine_ls_number_parameters     82
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0351
_refine_ls_wR_factor_ref         0.0731
_refine_ls_wR_factor_gt          0.0698
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.003

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
Eu1 Eu 1.14130(2) 1.14130(2) 0.14130(2) 0.01583(4) Uani 1 3 d S T P . .
O1 O 1.04850(13) 0.89311(13) 0.11198(14) 0.0406(7) Uani 1 1 d . . . . .
H1B H 1.0339 0.8493 0.1337 0.061 Uiso 1 1 calc R U . . .
O1W O 0.98341(15) 0.98341(15) -0.01659(15) 0.0588(13) Uani 1 3 d S T P . .
H1W H 0.9740 1.0303 -0.0399 0.071 Uiso 0.3333 1 d R U P . .
H2W H 0.9332 0.9677 -0.0190 0.071 Uiso 0.3333 1 d R U P . .
O2 O 1.15769(12) 1.00194(11) 0.12245(12) 0.0320(7) Uani 1 1 d . . . . .
O2W O 1.0000 0.7500 0.1840(2) 0.0785(15) Uani 1 2 d S TU P . .
H3W H 0.9703 0.7514 0.1402 0.094 Uiso 0.5 1 d R U P . .
H4W H 1.0092 0.7206 0.2270 0.094 Uiso 0.5 1 d R U P . .
O3 O 1.16041(13) 0.87590(12) 0.21870(12) 0.0374(7) Uani 1 1 d . . . . .
P1 P 1.14277(5) 0.91074(4) 0.13406(5) 0.02287(19) Uani 1 1 d . . . . .
C1 C 1.2500 0.8976(2) 0.0000 0.0237(11) Uani 1 2 d S TU P . .
H1A H 1.2500 0.9555 0.0000 0.028 Uiso 1 2 calc R U P . .
C2 C 1.20432(19) 0.85521(19) 0.05958(16) 0.0297(8) Uani 1 1 d . U . . .
C3 C 1.2058(2) 0.7684(2) 0.0593(2) 0.0531(10) Uani 1 1 d . U . . .
H3A H 1.1766 0.7389 0.0996 0.064 Uiso 1 1 calc R U . . .
C4 C 1.2500 0.7267(3) 0.0000 0.0686(13) Uani 1 2 d S TU P . .
C5 C 1.2500 0.6295(3) 0.0000 0.0879(17) Uani 1 2 d S TU P . .
H5A H 1.2553 0.6095 -0.0561 0.132 Uiso 0.5 1 calc R U P . .
H5B H 1.1988 0.6095 0.0234 0.132 Uiso 0.5 1 calc R U P . .
H5C H 1.2959 0.6095 0.0327 0.132 Uiso 0.5 1 calc R U P . .


_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
Eu1 O2 2.2748(18) . ?
Eu1 O2 2.2748(18) 5_654 ?
Eu1 O2 2.2748(18) 9_564 ?
Eu1 O3 2.2869(19) 16_465 ?
Eu1 O3 2.2869(19) 24_663 ?
Eu1 O3 2.2869(19) 20_645 ?
O1 P1 1.581(2) . ?
O2 P1 1.4964(19) . ?
O3 P1 1.498(2) . ?
O3 Eu1 2.2869(19) 16_465 ?
P1 C2 1.791(3) . ?
C1 C2 1.386(3) 15_744 ?
C1 C2 1.386(3) . ?
C2 C3 1.395(4) . ?
C3 C4 1.364(4) . ?
C4 C3 1.364(4) 15_744 ?
C4 C5 1.562(8) . ?

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
O2 Eu1 O2 89.90(7) . 5_654 ?
O2 Eu1 O2 89.90(7) . 9_564 ?
O2 Eu1 O2 89.90(7) 5_654 9_564 ?
O2 Eu1 O3 89.80(7) . 16_465 ?
O2 Eu1 O3 179.70(7) 5_654 16_465 ?
O2 Eu1 O3 90.12(7) 9_564 16_465 ?
O2 Eu1 O3 179.70(7) . 24_663 ?
O2 Eu1 O3 90.12(7) 5_654 24_663 ?
O2 Eu1 O3 89.80(7) 9_564 24_663 ?
O3 Eu1 O3 90.17(7) 16_465 24_663 ?
O2 Eu1 O3 90.12(7) . 20_645 ?
O2 Eu1 O3 89.80(7) 5_654 20_645 ?
O2 Eu1 O3 179.70(7) 9_564 20_645 ?
O3 Eu1 O3 90.17(7) 16_465 20_645 ?
O3 Eu1 O3 90.17(7) 24_663 20_645 ?
P1 O2 Eu1 158.22(12) . . ?
P1 O3 Eu1 155.90(13) . 16_465 ?
O2 P1 O3 116.67(11) . . ?
O2 P1 O1 107.52(12) . . ?
O3 P1 O1 108.54(12) . . ?
O2 P1 C2 108.43(13) . . ?
O3 P1 C2 108.42(13) . . ?
O1 P1 C2 106.85(13) . . ?
C2 C1 C2 121.0(4) 15_744 . ?
C1 C2 C3 118.7(3) . . ?
C1 C2 P1 120.6(2) . . ?
C3 C2 P1 120.7(2) . . ?
C4 C3 C2 120.2(3) . . ?
C3 C4 C3 121.1(5) 15_744 . ?
C3 C4 C5 119.5(2) 15_744 . ?
C3 C4 C5 119.5(2) . . ?

_refine_diff_density_max         0.512
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.097

_shelxl_version_number           2013-2

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1400188'
_audit_update_record             
;
2015-08-24 deposited with the CCDC.
2015-09-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H34 Gd2 O23 P6'
_chemical_formula_weight         1154.80

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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           199
_space_group_name_H-M_alt        'I 21 3'
_space_group_name_Hall           'I 2b 2c 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   16.0416(9)
_cell_length_b                   16.0416(9)
_cell_length_c                   16.0416(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4128.0(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       cubic
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.858
_exptl_crystal_F_000             2248
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    3.495
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.480
_exptl_absorpt_correction_T_max  0.485
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6288
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.111
_diffrn_reflns_theta_max         24.928
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.974
_reflns_number_total             1222
_reflns_number_gt                1096
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.794
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    0.978

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_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.
;
_vrf_PLAT417_2                   
;
PROBLEM: Short Inter D-H..H-D H1B .. H3W .. 1.62 Ang.
RESPONSE: O2W is situated at a special position (1.00 0.75 0.183707).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0273P)²+6.5066P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 450 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.034(14)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         1222
_refine_ls_number_parameters     82
_refine_ls_number_restraints     45
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0279
_refine_ls_wR_factor_ref         0.0595
_refine_ls_wR_factor_gt          0.0559
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.010

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
Gd1 Gd 1.14142(2) 1.14142(2) 0.14142(2) 0.01599(3) Uani 1 3 d S T P . .
O1 O 1.04921(11) 0.89325(12) 0.11319(12) 0.0414(6) Uani 1 1 d . . . . .
H1B H 1.0348 0.8494 0.1350 0.062 Uiso 1 1 calc R U . . .
O1W O 0.98241(14) 0.98241(14) -0.01759(14) 0.0605(11) Uani 1 3 d S T P . .
H1W H 0.9731 1.0303 -0.0399 0.073 Uiso 0.3333 1 d R U P . .
H2W H 0.9322 0.9677 -0.0190 0.073 Uiso 0.3333 1 d R U P . .
O2 O 1.15787(11) 1.00214(9) 0.12427(10) 0.0342(6) Uani 1 1 d . . . . .
O2W O 1.0000 0.7500 0.1835(2) 0.0773(12) Uani 1 2 d S TU P . .
H3W H 0.9703 0.7514 0.1398 0.093 Uiso 0.5 1 d R U P . .
H4W H 1.0092 0.7206 0.2266 0.093 Uiso 0.5 1 d R U P . .
O3 O 1.16045(11) 0.87576(10) 0.21913(10) 0.0357(6) Uani 1 1 d . . . . .
P1 P 1.14298(4) 0.91098(3) 0.13451(4) 0.02263(15) Uani 1 1 d . . . . .
C1 C 1.2500 0.8984(2) 0.0000 0.0246(11) Uani 1 2 d S T P . .
H1A H 1.2500 0.9564 0.0000 0.030 Uiso 1 2 calc R U P . .
C2 C 1.20472(16) 0.85761(17) 0.05999(14) 0.0306(7) Uani 1 1 d . U . . .
C3 C 1.2054(2) 0.76879(18) 0.0583(2) 0.0518(8) Uani 1 1 d . U . . .
H3A H 1.1747 0.7395 0.0978 0.062 Uiso 1 1 calc R U . . .
C4 C 1.2500 0.7257(3) 0.0000 0.0675(11) Uani 1 2 d S TU P . .
C5 C 1.2500 0.6284(3) 0.0000 0.0853(14) Uani 1 2 d S TU P . .
H5A H 1.2653 0.6084 -0.0543 0.128 Uiso 0.5 1 calc R U P . .
H5B H 1.1953 0.6084 0.0139 0.128 Uiso 0.5 1 calc R U P . .
H5C H 1.2894 0.6084 0.0404 0.128 Uiso 0.5 1 calc R U P . .


_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
Gd1 O2 2.2667(15) . ?
Gd1 O2 2.2667(15) 5_654 ?
Gd1 O2 2.2667(15) 9_564 ?
Gd1 O3 2.2744(16) 16_465 ?
Gd1 O3 2.2744(16) 24_663 ?
Gd1 O3 2.2744(16) 20_645 ?
O1 P1 1.5687(19) . ?
O2 P1 1.4907(16) . ?
O3 P1 1.4967(17) . ?
O3 Gd1 2.2744(16) 16_465 ?
P1 C2 1.773(3) . ?
C1 C2 1.372(3) 15_744 ?
C1 C2 1.372(3) . ?
C2 C3 1.425(4) . ?
C3 C4 1.366(4) . ?
C4 C3 1.366(4) 15_744 ?
C4 C5 1.561(7) . ?

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
O2 Gd1 O2 90.52(6) . 5_654 ?
O2 Gd1 O2 90.52(6) . 9_564 ?
O2 Gd1 O2 90.52(6) 5_654 9_564 ?
O2 Gd1 O3 89.10(6) . 16_465 ?
O2 Gd1 O3 179.21(6) 5_654 16_465 ?
O2 Gd1 O3 90.18(6) 9_564 16_465 ?
O2 Gd1 O3 179.20(6) . 24_663 ?
O2 Gd1 O3 90.18(6) 5_654 24_663 ?
O2 Gd1 O3 89.10(6) 9_564 24_663 ?
O3 Gd1 O3 90.20(6) 16_465 24_663 ?
O2 Gd1 O3 90.18(6) . 20_645 ?
O2 Gd1 O3 89.10(6) 5_654 20_645 ?
O2 Gd1 O3 179.21(6) 9_564 20_645 ?
O3 Gd1 O3 90.20(6) 16_465 20_645 ?
O3 Gd1 O3 90.20(6) 24_663 20_645 ?
P1 O2 Gd1 159.21(11) . . ?
P1 O3 Gd1 155.86(11) . 16_465 ?
O2 P1 O3 116.12(10) . . ?
O2 P1 O1 107.90(10) . . ?
O3 P1 O1 107.99(10) . . ?
O2 P1 C2 108.05(12) . . ?
O3 P1 C2 108.94(11) . . ?
O1 P1 C2 107.53(11) . . ?
C2 C1 C2 123.0(3) 15_744 . ?
C1 C2 C3 117.4(3) . . ?
C1 C2 P1 122.6(2) . . ?
C3 C2 P1 120.0(2) . . ?
C4 C3 C2 121.6(3) . . ?
C3 C4 C3 119.1(4) . 15_744 ?
C3 C4 C5 120.4(2) . . ?
C3 C4 C5 120.4(2) 15_744 . ?

_refine_diff_density_max         0.475
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.087

_shelxl_version_number           2013-2

####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1400189'
_audit_update_record             
;
2015-08-24 deposited with the CCDC.
2015-09-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H34 O23 P6 Tb2'
_chemical_formula_weight         1158.14

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'

_space_group_crystal_system      cubic
_space_group_IT_number           199
_space_group_name_H-M_alt        'I 21 3'
_space_group_name_Hall           'I 2b 2c 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   16.0134(11)
_cell_length_b                   16.0134(11)
_cell_length_c                   16.0134(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4106.3(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    297(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      3.116
_cell_measurement_theta_max      24.975

_exptl_crystal_description       cubic
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.873
_exptl_crystal_F_000             2256
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_exptl_absorpt_coefficient_mu    3.728
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.440
_exptl_absorpt_correction_T_max  0.458
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      297(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10160
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.116
_diffrn_reflns_theta_max         24.975
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             1219
_reflns_number_gt                1109
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.787
_reflns_Friedel_fraction_max     0.993
_reflns_Friedel_fraction_full    0.978

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_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.
;
_vrf_PLAT417_3                   
;
PROBLEM: Short Inter D-H..H-D H1B .. H3W .. 1.61 Ang.
RESPONSE: O2W is situated at a special position (0.00 0.25 0.816208).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0288P)²+63.1804P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 466 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.022(18)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         1219
_refine_ls_number_parameters     82
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0348
_refine_ls_wR_factor_ref         0.0868
_refine_ls_wR_factor_gt          0.0782
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_restrained_S_all      1.112
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001

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 -0.14116(2) -0.14116(2) 0.85884(2) 0.02054(4) Uani 1 3 d S T P . .
O1 O -0.04898(17) 0.10729(18) 0.88681(18) 0.0446(8) Uani 1 1 d . . . . .
H1B H -0.0348 0.1513 0.8648 0.067 Uiso 1 1 calc R U . . .
O1W O 0.0175(2) 0.0175(2) 1.0175(2) 0.0656(16) Uani 1 3 d S T P . .
H1W H 0.0268 -0.0303 1.0399 0.079 Uiso 0.3333 1 d R U P . .
H2W H 0.0677 0.0323 1.0190 0.079 Uiso 0.3333 1 d R U P . .
O2 O -0.15723(16) -0.00255(13) 0.87534(15) 0.0355(8) Uani 1 1 d . . . . .
O2W O 0.0000 0.2500 0.8162(3) 0.0763(16) Uani 1 2 d S TU P . .
H3W H 0.0297 0.2486 0.8600 0.092 Uiso 0.5 1 d R U P . .
H4W H -0.0092 0.2794 0.7732 0.092 Uiso 0.5 1 d R U P . .
O3 O -0.16052(17) 0.12393(16) 0.77981(15) 0.0406(8) Uani 1 1 d . . . . .
P1 P -0.14272(6) 0.08877(5) 0.86515(5) 0.0256(2) Uani 1 1 d . . . . .
C1 C -0.2500 0.1027(3) 1.0000 0.0290(14) Uani 1 2 d S T P . .
H1A H -0.2500 0.0447 1.0000 0.035 Uiso 1 2 calc R U P . .
C2 C -0.2047(2) 0.1437(2) 0.93987(19) 0.0294(9) Uani 1 1 d . . . . .
C3 C -0.2054(3) 0.2321(3) 0.9412(3) 0.0561(13) Uani 1 1 d . U . . .
H3A H -0.1751 0.2615 0.9013 0.067 Uiso 1 1 calc R U . . .
C4 C -0.2500 0.2747(4) 1.0000 0.0633(16) Uani 1 2 d S TU P . .
C5 C -0.2500 0.3706(5) 1.0000 0.090(2) Uani 1 2 d S TU P . .
H5A H -0.2974 0.3906 0.9692 0.135 Uiso 0.5 1 calc R U P . .
H5B H -0.1997 0.3906 0.9743 0.135 Uiso 0.5 1 calc R U P . .
H5C H -0.2529 0.3906 1.0564 0.135 Uiso 0.5 1 calc R U P . .


_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 O2 2.250(2) 9_546 ?
Tb1 O2 2.250(2) 5_456 ?
Tb1 O2 2.250(2) . ?
Tb1 O3 2.259(2) 20_545 ?
Tb1 O3 2.259(2) 16_446 ?
Tb1 O3 2.259(2) 24_455 ?
O1 P1 1.569(3) . ?
O2 P1 1.490(2) . ?
O3 P1 1.505(3) . ?
O3 Tb1 2.259(2) 16_446 ?
P1 C2 1.786(3) . ?
C1 C2 1.372(4) 15_446 ?
C1 C2 1.372(4) . ?
C2 C3 1.416(5) . ?
C3 C4 1.365(6) . ?
C4 C3 1.365(6) 15_446 ?
C4 C5 1.536(11) . ?

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
O2 Tb1 O2 90.60(9) 9_546 5_456 ?
O2 Tb1 O2 90.60(9) 9_546 . ?
O2 Tb1 O2 90.60(9) 5_456 . ?
O2 Tb1 O3 178.76(9) 9_546 20_545 ?
O2 Tb1 O3 88.81(9) 5_456 20_545 ?
O2 Tb1 O3 90.49(10) . 20_545 ?
O2 Tb1 O3 90.50(10) 9_546 16_446 ?
O2 Tb1 O3 178.76(9) 5_456 16_446 ?
O2 Tb1 O3 88.81(9) . 16_446 ?
O3 Tb1 O3 90.10(9) 20_545 16_446 ?
O2 Tb1 O3 88.81(9) 9_546 24_455 ?
O2 Tb1 O3 90.50(10) 5_456 24_455 ?
O2 Tb1 O3 178.76(10) . 24_455 ?
O3 Tb1 O3 90.10(9) 20_545 24_455 ?
O3 Tb1 O3 90.10(9) 16_446 24_455 ?
P1 O2 Tb1 159.67(16) . . ?
P1 O3 Tb1 155.80(17) . 16_446 ?
O2 P1 O3 115.91(15) . . ?
O2 P1 O1 108.10(15) . . ?
O3 P1 O1 108.13(16) . . ?
O2 P1 C2 108.87(16) . . ?
O3 P1 C2 108.58(15) . . ?
O1 P1 C2 106.89(16) . . ?
C2 C1 C2 122.9(5) 15_446 . ?
C1 C2 C3 117.6(4) . . ?
C1 C2 P1 121.9(3) . . ?
C3 C2 P1 120.4(3) . . ?
C4 C3 C2 121.0(4) . . ?
C3 C4 C3 120.0(6) 15_446 . ?
C3 C4 C5 120.0(3) 15_446 . ?
C3 C4 C5 120.0(3) . . ?

_refine_diff_density_max         1.358
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.117

_shelxl_version_number           2013-2

