# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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 1888860'
loop_
_audit_author_name
_audit_author_address
'Colin McMillen'
;Clemson University
United States of America
;
_audit_update_record             
;
2019-01-04 deposited with the CCDC.	2019-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'H La2 Nb O6'
_chemical_formula_weight         467.74

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.0987(17)
_cell_length_b                   6.8056(18)
_cell_length_c                   10.259(3)
_cell_angle_alpha                90
_cell_angle_beta                 94.345(9)
_cell_angle_gamma                90
_cell_volume                     494.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2829
_cell_measurement_theta_min      2.99
_cell_measurement_theta_max      26.01

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    .
_exptl_crystal_density_diffrn    6.286
_exptl_crystal_F_000             816
_exptl_transmission_factor_min   .
_exptl_transmission_factor_max   .
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    19.203
_shelx_estimated_absorpt_T_min   0.207
_shelx_estimated_absorpt_T_max   0.392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8691
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'REQAB, CrystalClear'
_exptl_absorpt_special_details   .
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine focus sealed tube'
_diffrn_measurement_device_type  'Mercury CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean .
_diffrn_reflns_number            4022
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.374
_diffrn_reflns_theta_max         25.225
_diffrn_reflns_theta_full        25.225
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             899
_reflns_number_gt                864
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       'Rigaku CrystalClear, 2014'
_computing_cell_refinement       'Rigaku CrystalClear, 2014'
_computing_data_reduction        'Rigaku CrystalClear, 2014'
_computing_structure_solution    'SHELXT-2014 (Sheldrick 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND (Bradenburg, 1999)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0315P)²+3.8933P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.0217(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         899
_refine_ls_number_parameters     86
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0247
_refine_ls_wR_factor_ref         0.0585
_refine_ls_wR_factor_gt          0.0580
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_restrained_S_all      1.148
_refine_ls_shift/su_max          0.000
_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_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
La1 La -0.36920(5) 0.08133(5) 0.21060(4) 0.00884(19) Uani 1 1 d . . . . .
La2 La 0.11966(5) 0.23448(6) 0.08292(4) 0.00927(19) Uani 1 1 d . . . . .
Nb1 Nb 0.13492(8) 0.15424(9) 0.42748(6) 0.0075(2) Uani 1 1 d . . . . .
O1 O -0.0482(7) 0.1514(7) 0.5746(5) 0.0099(10) Uani 1 1 d . . . . .
O2 O 0.2944(7) 0.0803(7) 0.2905(5) 0.0113(10) Uani 1 1 d . . . . .
O3 O -0.0621(7) 0.2331(7) 0.2920(5) 0.0112(10) Uani 1 1 d . . . . .
O4 O 0.0704(7) 0.1122(8) -0.1431(5) 0.0135(11) Uani 1 1 d D . . . .
H4 H -0.049(6) 0.092(13) -0.183(8) 0.020 Uiso 1 1 d D U . . .
O5 O 0.3327(7) 0.0514(8) 0.5610(5) 0.0133(10) Uani 1 1 d . . . . .
O6 O 0.1949(8) 0.4155(7) 0.4697(5) 0.0173(12) 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
La1 O3 2.419(5) 2_445 ?
La1 O3 2.498(5) . ?
La1 O5 2.506(5) 3_556 ?
La1 O6 2.547(5) 4_565 ?
La1 O1 2.569(5) 4_565 ?
La1 O2 2.583(5) 1_455 ?
La1 O4 2.623(5) 4_566 ?
La1 O4 2.633(5) 3 ?
La1 Nb1 3.4189(10) 4_565 ?
La1 Nb1 3.6890(10) 2_445 ?
La1 La2 3.7136(8) 2_445 ?
La1 La1 3.8587(9) 2_455 ?
La2 O4 2.464(5) . ?
La2 O1 2.490(5) 4_665 ?
La2 O5 2.501(5) 4_565 ?
La2 O3 2.586(5) . ?
La2 O2 2.603(5) . ?
La2 O6 2.616(5) 2_545 ?
La2 O5 2.650(5) 2 ?
La2 O2 2.734(5) 2 ?
La2 O4 2.810(5) 3 ?
La2 Nb1 3.3519(10) 2 ?
La2 Nb1 3.5704(12) . ?
Nb1 O6 1.871(5) . ?
Nb1 O2 1.936(5) . ?
Nb1 O3 1.970(5) . ?
Nb1 O5 2.011(5) . ?
Nb1 O1 2.066(5) . ?
Nb1 O1 2.169(5) 3_556 ?
Nb1 Nb1 3.2745(13) 3_556 ?
O4 H4 0.93(2) . ?

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
O3 La1 O3 125.37(14) 2_445 . ?
O3 La1 O5 70.36(17) 2_445 3_556 ?
O3 La1 O5 79.08(16) . 3_556 ?
O3 La1 O6 92.77(17) 2_445 4_565 ?
O3 La1 O6 96.04(18) . 4_565 ?
O5 La1 O6 153.76(17) 3_556 4_565 ?
O3 La1 O1 126.62(16) 2_445 4_565 ?
O3 La1 O1 105.78(15) . 4_565 ?
O5 La1 O1 140.77(16) 3_556 4_565 ?
O6 La1 O1 65.45(16) 4_565 4_565 ?
O3 La1 O2 79.07(16) 2_445 1_455 ?
O3 La1 O2 134.37(16) . 1_455 ?
O5 La1 O2 74.63(16) 3_556 1_455 ?
O6 La1 O2 123.07(17) 4_565 1_455 ?
O1 La1 O2 75.11(15) 4_565 1_455 ?
O3 La1 O4 138.03(16) 2_445 4_566 ?
O3 La1 O4 69.89(16) . 4_566 ?
O5 La1 O4 76.20(17) 3_556 4_566 ?
O6 La1 O4 126.67(15) 4_565 4_566 ?
O1 La1 O4 69.65(15) 4_565 4_566 ?
O2 La1 O4 68.01(15) 1_455 4_566 ?
O3 La1 O4 70.90(17) 2_445 3 ?
O3 La1 O4 66.11(16) . 3 ?
O5 La1 O4 92.13(16) 3_556 3 ?
O6 La1 O4 62.77(16) 4_565 3 ?
O1 La1 O4 125.91(15) 4_565 3 ?
O2 La1 O4 149.82(16) 1_455 3 ?
O4 La1 O4 135.87(10) 4_566 3 ?
O3 La1 Nb1 121.39(12) 2_445 4_565 ?
O3 La1 Nb1 90.17(11) . 4_565 ?
O5 La1 Nb1 167.69(12) 3_556 4_565 ?
O6 La1 Nb1 32.58(11) 4_565 4_565 ?
O1 La1 Nb1 37.04(11) 4_565 4_565 ?
O2 La1 Nb1 109.80(11) 1_455 4_565 ?
O4 La1 Nb1 94.58(11) 4_566 4_565 ?
O4 La1 Nb1 88.91(11) 3 4_565 ?
O3 La1 Nb1 29.20(12) 2_445 2_445 ?
O3 La1 Nb1 149.55(11) . 2_445 ?
O5 La1 Nb1 95.09(12) 3_556 2_445 ?
O6 La1 Nb1 75.99(13) 4_565 2_445 ?
O1 La1 Nb1 97.58(11) 4_565 2_445 ?
O2 La1 Nb1 70.23(11) 1_455 2_445 ?
O4 La1 Nb1 138.17(11) 4_566 2_445 ?
O4 La1 Nb1 84.46(11) 3 2_445 ?
Nb1 La1 Nb1 97.21(2) 4_565 2_445 ?
O3 La1 La2 43.85(12) 2_445 2_445 ?
O3 La1 La2 121.03(12) . 2_445 ?
O5 La1 La2 42.08(11) 3_556 2_445 ?
O6 La1 La2 133.43(12) 4_565 2_445 ?
O1 La1 La2 121.41(10) 4_565 2_445 ?
O2 La1 La2 47.40(11) 1_455 2_445 ?
O4 La1 La2 94.18(11) 4_566 2_445 ?
O4 La1 La2 105.18(12) 3 2_445 ?
Nb1 La1 La2 148.702(18) 4_565 2_445 ?
Nb1 La1 La2 57.672(19) 2_445 2_445 ?
O3 La1 La1 161.99(12) 2_445 2_455 ?
O3 La1 La1 37.58(11) . 2_455 ?
O5 La1 La1 96.27(12) 3_556 2_455 ?
O6 La1 La1 95.05(12) 4_565 2_455 ?
O1 La1 La1 71.37(11) 4_565 2_455 ?
O2 La1 La1 109.70(10) 1_455 2_455 ?
O4 La1 La1 42.88(11) 4_566 2_455 ?
O4 La1 La1 98.46(11) 3 2_455 ?
Nb1 La1 La1 71.46(2) 4_565 2_455 ?
Nb1 La1 La1 168.149(19) 2_445 2_455 ?
La2 La1 La1 131.48(2) 2_445 2_455 ?
O4 La2 O1 98.07(16) . 4_665 ?
O4 La2 O5 93.19(16) . 4_565 ?
O1 La2 O5 125.60(16) 4_665 4_565 ?
O4 La2 O3 137.37(16) . . ?
O1 La2 O3 124.24(15) 4_665 . ?
O5 La2 O3 67.82(16) 4_565 . ?
O4 La2 O2 131.22(16) . . ?
O1 La2 O2 76.11(15) 4_665 . ?
O5 La2 O2 130.00(15) 4_565 . ?
O3 La2 O2 63.67(15) . . ?
O4 La2 O6 64.11(16) . 2_545 ?
O1 La2 O6 76.07(17) 4_665 2_545 ?
O5 La2 O6 152.14(17) 4_565 2_545 ?
O3 La2 O6 117.30(15) . 2_545 ?
O2 La2 O6 67.56(15) . 2_545 ?
O4 La2 O5 76.43(16) . 2 ?
O1 La2 O5 64.27(15) 4_665 2 ?
O5 La2 O5 67.24(19) 4_565 2 ?
O3 La2 O5 123.92(15) . 2 ?
O2 La2 O5 135.31(15) . 2 ?
O6 La2 O5 118.23(15) 2_545 2 ?
O4 La2 O2 138.43(16) . 2 ?
O1 La2 O2 64.52(15) 4_665 2 ?
O5 La2 O2 72.07(16) 4_565 2 ?
O3 La2 O2 73.54(15) . 2 ?
O2 La2 O2 83.29(7) . 2 ?
O6 La2 O2 135.60(17) 2_545 2 ?
O5 La2 O2 62.01(15) 2 2 ?
O4 La2 O4 83.52(16) . 3 ?
O1 La2 O4 137.83(15) 4_665 3 ?
O5 La2 O4 96.18(16) 4_565 3 ?
O3 La2 O4 62.40(15) . 3 ?
O2 La2 O4 71.86(14) . 3 ?
O6 La2 O4 66.79(17) 2_545 3 ?
O5 La2 O4 152.82(15) 2 3 ?
O2 La2 O4 135.40(14) 2 3 ?
O4 La2 Nb1 107.15(12) . 2 ?
O1 La2 Nb1 40.30(11) 4_665 2 ?
O5 La2 Nb1 85.54(12) 4_565 2 ?
O3 La2 Nb1 108.82(11) . 2 ?
O2 La2 Nb1 98.80(11) . 2 ?
O6 La2 Nb1 115.46(13) 2_545 2 ?
O5 La2 Nb1 36.87(10) 2 2 ?
O2 La2 Nb1 35.28(10) 2 2 ?
O4 La2 Nb1 169.13(10) 3 2 ?
O4 La2 Nb1 150.67(13) . . ?
O1 La2 Nb1 97.10(11) 4_665 . ?
O5 La2 Nb1 98.14(12) 4_565 . ?
O3 La2 Nb1 32.61(11) . . ?
O2 La2 Nb1 31.93(10) . . ?
O6 La2 Nb1 95.69(11) 2_545 . ?
O5 La2 Nb1 132.89(11) 2 . ?
O2 La2 Nb1 70.89(10) 2 . ?
O4 La2 Nb1 68.47(10) 3 . ?
Nb1 La2 Nb1 100.663(17) 2 . ?
O4 La2 La1 135.38(12) . 2_455 ?
O1 La2 La1 108.46(11) 4_665 2_455 ?
O5 La2 La1 42.19(11) 4_565 2_455 ?
O3 La2 La1 40.40(11) . 2_455 ?
O2 La2 La1 90.48(10) . 2_455 ?
O6 La2 La1 156.23(11) 2_545 2_455 ?
O5 La2 La1 83.54(11) 2 2_455 ?
O2 La2 La1 44.06(10) 2 2_455 ?
O4 La2 La1 98.61(10) 3 2_455 ?
Nb1 La2 La1 75.46(2) 2 2_455 ?
Nb1 La2 La1 60.816(18) . 2_455 ?
O6 Nb1 O2 106.2(2) . . ?
O6 Nb1 O3 92.4(2) . . ?
O2 Nb1 O3 88.9(2) . . ?
O6 Nb1 O5 92.2(2) . . ?
O2 Nb1 O5 89.3(2) . . ?
O3 Nb1 O5 175.4(2) . . ?
O6 Nb1 O1 89.1(2) . . ?
O2 Nb1 O1 164.3(2) . . ?
O3 Nb1 O1 93.8(2) . . ?
O5 Nb1 O1 86.81(19) . . ?
O6 Nb1 O1 166.6(2) . 3_556 ?
O2 Nb1 O1 85.67(19) . 3_556 ?
O3 Nb1 O1 93.93(19) . 3_556 ?
O5 Nb1 O1 81.71(19) . 3_556 ?
O1 Nb1 O1 78.73(19) . 3_556 ?
O6 Nb1 Nb1 129.40(17) . 3_556 ?
O2 Nb1 Nb1 123.88(14) . 3_556 ?
O3 Nb1 Nb1 94.99(15) . 3_556 ?
O5 Nb1 Nb1 82.50(14) . 3_556 ?
O1 Nb1 Nb1 40.51(13) . 3_556 ?
O1 Nb1 Nb1 38.22(12) 3_556 3_556 ?
O6 Nb1 La2 135.02(18) . 2_545 ?
O2 Nb1 La2 54.67(14) . 2_545 ?
O3 Nb1 La2 123.55(14) . 2_545 ?
O5 Nb1 La2 52.23(16) . 2_545 ?
O1 Nb1 La2 111.89(13) . 2_545 ?
O1 Nb1 La2 47.94(12) 3_556 2_545 ?
Nb1 Nb1 La2 77.96(3) 3_556 2_545 ?
O6 Nb1 La1 47.14(15) . 4_666 ?
O2 Nb1 La1 142.78(15) . 4_666 ?
O3 Nb1 La1 113.86(15) . 4_666 ?
O5 Nb1 La1 69.82(15) . 4_666 ?
O1 Nb1 La1 48.52(13) . 4_666 ?
O1 Nb1 La1 119.52(12) 3_556 4_666 ?
Nb1 Nb1 La1 84.75(3) 3_556 4_666 ?
La2 Nb1 La1 120.90(2) 2_545 4_666 ?
O6 Nb1 La2 94.19(16) . . ?
O2 Nb1 La2 45.32(15) . . ?
O3 Nb1 La2 45.02(15) . . ?
O5 Nb1 La2 134.01(15) . . ?
O1 Nb1 La2 138.72(13) . . ?
O1 Nb1 La2 98.59(12) 3_556 . ?
Nb1 Nb1 La2 124.96(3) 3_556 . ?
La2 Nb1 La2 94.341(17) 2_545 . ?
La1 Nb1 La2 139.38(2) 4_666 . ?
O6 Nb1 La1 56.02(17) . 2_455 ?
O2 Nb1 La1 103.65(14) . 2_455 ?
O3 Nb1 La1 36.81(14) . 2_455 ?
O5 Nb1 La1 147.77(16) . 2_455 ?
O1 Nb1 La1 87.49(13) . 2_455 ?
O1 Nb1 La1 127.98(12) 3_556 2_455 ?
Nb1 Nb1 La1 112.33(3) 3_556 2_455 ?
La2 Nb1 La1 155.67(2) 2_545 2_455 ?
La1 Nb1 La1 82.79(2) 4_666 2_455 ?
La2 Nb1 La1 61.511(14) . 2_455 ?
O6 Nb1 La2 61.67(18) . 4_666 ?
O2 Nb1 La2 78.08(15) . 4_666 ?
O3 Nb1 La2 145.34(14) . 4_666 ?
O5 Nb1 La2 37.99(14) . 4_666 ?
O1 Nb1 La2 107.36(13) . 4_666 ?
O1 Nb1 La2 116.58(12) 3_556 4_666 ?
Nb1 Nb1 La2 118.99(3) 3_556 4_666 ?
La2 Nb1 La2 73.97(2) 2_545 4_666 ?
La1 Nb1 La2 66.419(17) 4_666 4_666 ?
La2 Nb1 La2 110.33(2) . 4_666 ?
La1 Nb1 La2 115.42(2) 2_455 4_666 ?
Nb1 O1 Nb1 101.27(19) . 3_556 ?
Nb1 O1 La2 132.2(2) . 4_566 ?
Nb1 O1 La2 91.76(17) 3_556 4_566 ?
Nb1 O1 La1 94.44(18) . 4_666 ?
Nb1 O1 La1 144.4(2) 3_556 4_666 ?
La2 O1 La1 101.03(16) 4_566 4_666 ?
Nb1 O2 La1 146.6(2) . 1_655 ?
Nb1 O2 La2 102.7(2) . . ?
La1 O2 La2 97.69(16) 1_655 . ?
Nb1 O2 La2 90.05(17) . 2_545 ?
La1 O2 La2 88.54(15) 1_655 2_545 ?
La2 O2 La2 144.2(2) . 2_545 ?
Nb1 O3 La1 114.0(2) . 2_455 ?
Nb1 O3 La1 132.7(2) . . ?
La1 O3 La1 103.37(18) 2_455 . ?
Nb1 O3 La2 102.4(2) . . ?
La1 O3 La2 95.75(17) 2_455 . ?
La1 O3 La2 101.64(18) . . ?
La2 O4 La1 104.62(18) . 4_665 ?
La2 O4 La1 110.90(18) . 3 ?
La1 O4 La1 94.45(16) 4_665 3 ?
La2 O4 La2 96.48(16) . 3 ?
La1 O4 La2 153.53(19) 4_665 3 ?
La1 O4 La2 92.72(16) 3 3 ?
La2 O4 H4 122(6) . . ?
La1 O4 H4 93(6) 4_665 . ?
La1 O4 H4 123(6) 3 . ?
La2 O4 H4 62(6) 3 . ?
Nb1 O5 La2 112.3(2) . 4_666 ?
Nb1 O5 La1 141.2(2) . 3_556 ?
La2 O5 La1 95.74(16) 4_666 3_556 ?
Nb1 O5 La2 90.91(18) . 2_545 ?
La2 O5 La2 112.76(19) 4_666 2_545 ?
La1 O5 La2 102.66(18) 3_556 2_545 ?
Nb1 O6 La1 100.3(2) . 4_666 ?
Nb1 O6 La2 148.2(3) . 2 ?
La1 O6 La2 108.82(18) 4_666 2 ?

_refine_diff_density_max         1.249
_refine_diff_density_min         -2.508
_refine_diff_density_rms         0.378

####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1888864'
loop_
_audit_author_name
_audit_author_address
'Colin McMillen'
;Clemson University
United States of America
;
_audit_update_record             
;
2019-01-04 deposited with the CCDC.	2019-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'H Nd3 O10 Ta2'
_chemical_formula_weight         955.63

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_H-M_alt        'P n n m'
_space_group_name_Hall           '-P 2 2n'

_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, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   19.3122(8)
_cell_length_b                   5.5525(2)
_cell_length_c                   7.6800(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     823.53(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9426
_cell_measurement_theta_min      2.85
_cell_measurement_theta_max      30.68

_exptl_crystal_description       column
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    .
_exptl_crystal_density_diffrn    7.708
_exptl_crystal_F_000             1628
_exptl_transmission_factor_min   .
_exptl_transmission_factor_max   .
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    45.086
_shelx_estimated_absorpt_T_min   0.093
_shelx_estimated_absorpt_T_max   0.173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2760
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'SADABS, Bruker'
_exptl_absorpt_special_details   .
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   Ius
_diffrn_measurement_device_type  'Bruker Photon 100'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean .
_diffrn_reflns_number            11500
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.854
_diffrn_reflns_theta_max         25.489
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             827
_reflns_number_gt                778
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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 APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT-2014 (Sheldrick 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND (Bradenburg, 1999)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0285P)²+3.0564P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.00368(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         827
_refine_ls_number_parameters     79
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0214
_refine_ls_wR_factor_ref         0.0509
_refine_ls_wR_factor_gt          0.0501
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_restrained_S_all      1.176
_refine_ls_shift/su_max          0.000
_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_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
Nd1 Nd 0.14247(3) 0.42229(11) 0.000000 0.01827(19) Uani 1 2 d S T P . .
Nd2 Nd 0.09630(3) -0.50919(11) 0.500000 0.01790(19) Uani 1 2 d S T P . .
Nd3 Nd 0.000000 0.000000 0.25782(7) 0.01845(19) Uani 1 2 d S T P . .
Ta1 Ta 0.18267(2) -0.07989(6) 0.25183(3) 0.01658(15) Uani 1 1 d . . . . .
O1 O 0.2682(3) 0.0986(10) 0.3032(7) 0.0190(11) Uani 1 1 d . . . . .
O2 O -0.0022(4) -0.7444(14) 0.500000 0.0200(17) Uani 1 2 d S T P . .
O3 O 0.1782(4) -0.1783(14) 0.500000 0.0193(17) Uani 1 2 d S T P . .
O4 O 0.1221(3) 0.1906(10) 0.2799(6) 0.0190(12) Uani 1 1 d . . . . .
O5 O 0.0995(3) -0.2848(10) 0.2124(7) 0.0185(12) Uani 1 1 d . . . . .
O6 O 0.0273(4) 0.2553(13) 0.000000 0.0213(17) Uani 1 2 d DS T P . .
H6 H 0.045850 0.099463 0.000000 0.020 Uiso 1 2 d DS U P . .
O7 O 0.1888(4) 0.0078(14) 0.000000 0.0199(17) Uani 1 2 d S T 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
Nd1 O6 2.410(8) . ?
Nd1 O5 2.449(5) 1_565 ?
Nd1 O5 2.449(5) 6_565 ?
Nd1 O7 2.469(8) . ?
Nd1 O1 2.494(6) 3 ?
Nd1 O1 2.494(6) 8_665 ?
Nd1 O4 2.536(5) . ?
Nd1 O4 2.536(5) 6 ?
Nd1 Ta1 3.4617(6) 1_565 ?
Nd1 Ta1 3.4617(6) 6_565 ?
Nd1 Ta1 3.4811(6) 6 ?
Nd1 Ta1 3.4811(6) . ?
Nd2 O2 2.299(8) 5_546 ?
Nd2 O2 2.308(8) . ?
Nd2 O3 2.424(8) . ?
Nd2 O4 2.426(5) 1_545 ?
Nd2 O4 2.426(5) 6_546 ?
Nd2 O5 2.536(6) 6_556 ?
Nd2 O5 2.536(6) . ?
Nd2 Ta1 3.4780(6) 6_556 ?
Nd2 Ta1 3.4780(6) . ?
Nd2 Nd2 3.7209(12) 5_546 ?
Nd2 Nd3 3.7874(6) 1_545 ?
Nd2 Nd3 3.7874(6) 5_546 ?
Nd3 O2 2.340(5) 1_565 ?
Nd3 O2 2.340(5) 5_546 ?
Nd3 O6 2.491(5) 5 ?
Nd3 O6 2.491(5) . ?
Nd3 O5 2.513(6) . ?
Nd3 O5 2.513(6) 2 ?
Nd3 O4 2.590(6) 2 ?
Nd3 O4 2.590(6) . ?
Nd3 Ta1 3.5557(4) 2 ?
Nd3 Ta1 3.5558(4) . ?
Nd3 Nd3 3.7199(11) 5_556 ?
Ta1 O4 1.916(5) . ?
Ta1 O1 1.967(5) . ?
Ta1 O3 1.985(2) . ?
Ta1 O5 1.992(5) . ?
Ta1 O7 1.998(2) . ?
Ta1 O1 2.065(5) 3_545 ?

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
O6 Nd1 O5 86.70(19) . 1_565 ?
O6 Nd1 O5 86.70(19) . 6_565 ?
O5 Nd1 O5 83.6(3) 1_565 6_565 ?
O6 Nd1 O7 88.6(3) . . ?
O5 Nd1 O7 137.89(13) 1_565 . ?
O5 Nd1 O7 137.89(13) 6_565 . ?
O6 Nd1 O1 142.13(13) . 3 ?
O5 Nd1 O1 64.52(18) 1_565 3 ?
O5 Nd1 O1 112.19(18) 6_565 3 ?
O7 Nd1 O1 96.64(19) . 3 ?
O6 Nd1 O1 142.13(13) . 8_665 ?
O5 Nd1 O1 112.19(18) 1_565 8_665 ?
O5 Nd1 O1 64.52(18) 6_565 8_665 ?
O7 Nd1 O1 96.64(19) . 8_665 ?
O1 Nd1 O1 74.6(3) 3 8_665 ?
O6 Nd1 O4 70.22(15) . . ?
O5 Nd1 O4 73.70(18) 1_565 . ?
O5 Nd1 O4 148.11(18) 6_565 . ?
O7 Nd1 O4 65.38(14) . . ?
O1 Nd1 O4 78.03(17) 3 . ?
O1 Nd1 O4 145.13(19) 8_665 . ?
O6 Nd1 O4 70.22(15) . 6 ?
O5 Nd1 O4 148.11(18) 1_565 6 ?
O5 Nd1 O4 73.70(18) 6_565 6 ?
O7 Nd1 O4 65.38(14) . 6 ?
O1 Nd1 O4 145.13(19) 3 6 ?
O1 Nd1 O4 78.03(17) 8_665 6 ?
O4 Nd1 O4 115.9(2) . 6 ?
O6 Nd1 Ta1 120.94(14) . 1_565 ?
O5 Nd1 Ta1 34.26(13) 1_565 1_565 ?
O5 Nd1 Ta1 85.30(13) 6_565 1_565 ?
O7 Nd1 Ta1 131.54(13) . 1_565 ?
O1 Nd1 Ta1 36.17(12) 3 1_565 ?
O1 Nd1 Ta1 82.54(12) 8_665 1_565 ?
O4 Nd1 Ta1 88.06(12) . 1_565 ?
O4 Nd1 Ta1 155.99(12) 6 1_565 ?
O6 Nd1 Ta1 120.94(14) . 6_565 ?
O5 Nd1 Ta1 85.30(13) 1_565 6_565 ?
O5 Nd1 Ta1 34.26(13) 6_565 6_565 ?
O7 Nd1 Ta1 131.54(13) . 6_565 ?
O1 Nd1 Ta1 82.54(12) 3 6_565 ?
O1 Nd1 Ta1 36.17(12) 8_665 6_565 ?
O4 Nd1 Ta1 155.99(12) . 6_565 ?
O4 Nd1 Ta1 88.06(12) 6 6_565 ?
Ta1 Nd1 Ta1 67.932(15) 1_565 6_565 ?
O6 Nd1 Ta1 84.13(15) . 6 ?
O5 Nd1 Ta1 167.89(13) 1_565 6 ?
O5 Nd1 Ta1 103.73(13) 6_565 6 ?
O7 Nd1 Ta1 34.17(3) . 6 ?
O1 Nd1 Ta1 119.81(13) 3 6 ?
O1 Nd1 Ta1 79.83(12) 8_665 6 ?
O4 Nd1 Ta1 95.70(12) . 6 ?
O4 Nd1 Ta1 32.58(12) 6 6 ?
Ta1 Nd1 Ta1 154.16(2) 1_565 6 ?
Ta1 Nd1 Ta1 106.212(10) 6_565 6 ?
O6 Nd1 Ta1 84.13(15) . . ?
O5 Nd1 Ta1 103.73(13) 1_565 . ?
O5 Nd1 Ta1 167.89(13) 6_565 . ?
O7 Nd1 Ta1 34.17(3) . . ?
O1 Nd1 Ta1 79.83(12) 3 . ?
O1 Nd1 Ta1 119.81(13) 8_665 . ?
O4 Nd1 Ta1 32.58(12) . . ?
O4 Nd1 Ta1 95.70(12) 6 . ?
Ta1 Nd1 Ta1 106.211(10) 1_565 . ?
Ta1 Nd1 Ta1 154.16(2) 6_565 . ?
Ta1 Nd1 Ta1 67.503(15) 6 . ?
O2 Nd2 O2 72.2(3) 5_546 . ?
O2 Nd2 O3 92.9(3) 5_546 . ?
O2 Nd2 O3 165.2(3) . . ?
O2 Nd2 O4 125.68(17) 5_546 1_545 ?
O2 Nd2 O4 77.31(19) . 1_545 ?
O3 Nd2 O4 112.76(19) . 1_545 ?
O2 Nd2 O4 125.68(17) 5_546 6_546 ?
O2 Nd2 O4 77.31(19) . 6_546 ?
O3 Nd2 O4 112.76(19) . 6_546 ?
O4 Nd2 O4 88.3(2) 1_545 6_546 ?
O2 Nd2 O5 73.64(15) 5_546 6_556 ?
O2 Nd2 O5 107.33(14) . 6_556 ?
O3 Nd2 O5 67.17(14) . 6_556 ?
O4 Nd2 O5 159.94(18) 1_545 6_556 ?
O4 Nd2 O5 74.09(17) 6_546 6_556 ?
O2 Nd2 O5 73.64(15) 5_546 . ?
O2 Nd2 O5 107.33(15) . . ?
O3 Nd2 O5 67.17(14) . . ?
O4 Nd2 O5 74.09(17) 1_545 . ?
O4 Nd2 O5 159.94(18) 6_546 . ?
O5 Nd2 O5 121.1(2) 6_556 . ?
O2 Nd2 Ta1 87.66(16) 5_546 6_556 ?
O2 Nd2 Ta1 141.56(9) . 6_556 ?
O3 Nd2 Ta1 33.66(3) . 6_556 ?
O4 Nd2 Ta1 138.97(14) 1_545 6_556 ?
O4 Nd2 Ta1 89.47(13) 6_546 6_556 ?
O5 Nd2 Ta1 34.37(12) 6_556 6_556 ?
O5 Nd2 Ta1 97.41(12) . 6_556 ?
O2 Nd2 Ta1 87.66(16) 5_546 . ?
O2 Nd2 Ta1 141.56(9) . . ?
O3 Nd2 Ta1 33.66(3) . . ?
O4 Nd2 Ta1 89.47(13) 1_545 . ?
O4 Nd2 Ta1 138.97(14) 6_546 . ?
O5 Nd2 Ta1 97.41(12) 6_556 . ?
O5 Nd2 Ta1 34.37(12) . . ?
Ta1 Nd2 Ta1 66.459(15) 6_556 . ?
O2 Nd2 Nd2 36.2(2) 5_546 5_546 ?
O2 Nd2 Nd2 36.0(2) . 5_546 ?
O3 Nd2 Nd2 129.14(19) . 5_546 ?
O4 Nd2 Nd2 102.95(14) 1_545 5_546 ?
O4 Nd2 Nd2 102.95(14) 6_546 5_546 ?
O5 Nd2 Nd2 90.62(13) 6_556 5_546 ?
O5 Nd2 Nd2 90.61(13) . 5_546 ?
Ta1 Nd2 Nd2 117.42(2) 6_556 5_546 ?
Ta1 Nd2 Nd2 117.43(2) . 5_546 ?
O2 Nd2 Nd3 93.02(17) 5_546 1_545 ?
O2 Nd2 Nd3 35.70(11) . 1_545 ?
O3 Nd2 Nd3 149.96(4) . 1_545 ?
O4 Nd2 Nd3 42.62(14) 1_545 1_545 ?
O4 Nd2 Nd3 87.05(13) 6_546 1_545 ?
O5 Nd2 Nd3 142.46(12) 6_556 1_545 ?
O5 Nd2 Nd3 86.43(12) . 1_545 ?
Ta1 Nd2 Nd3 176.139(13) 6_556 1_545 ?
Ta1 Nd2 Nd3 117.356(9) . 1_545 ?
Nd2 Nd2 Nd3 61.894(15) 5_546 1_545 ?
O2 Nd2 Nd3 93.02(17) 5_546 5_546 ?
O2 Nd2 Nd3 35.70(11) . 5_546 ?
O3 Nd2 Nd3 149.96(4) . 5_546 ?
O4 Nd2 Nd3 87.05(13) 1_545 5_546 ?
O4 Nd2 Nd3 42.62(14) 6_546 5_546 ?
O5 Nd2 Nd3 86.43(12) 6_556 5_546 ?
O5 Nd2 Nd3 142.46(12) . 5_546 ?
Ta1 Nd2 Nd3 117.356(9) 6_556 5_546 ?
Ta1 Nd2 Nd3 176.140(13) . 5_546 ?
Nd2 Nd2 Nd3 61.894(15) 5_546 5_546 ?
Nd3 Nd2 Nd3 58.823(17) 1_545 5_546 ?
O2 Nd3 O2 74.7(3) 1_565 5_546 ?
O2 Nd3 O6 166.6(3) 1_565 5 ?
O2 Nd3 O6 106.9(2) 5_546 5 ?
O2 Nd3 O6 106.9(2) 1_565 . ?
O2 Nd3 O6 166.6(3) 5_546 . ?
O6 Nd3 O6 74.7(3) 5 . ?
O2 Nd3 O5 120.4(2) 1_565 . ?
O2 Nd3 O5 73.4(2) 5_546 . ?
O6 Nd3 O5 72.1(2) 5 . ?
O6 Nd3 O5 95.0(2) . . ?
O2 Nd3 O5 73.4(2) 1_565 2 ?
O2 Nd3 O5 120.4(2) 5_546 2 ?
O6 Nd3 O5 95.0(2) 5 2 ?
O6 Nd3 O5 72.1(2) . 2 ?
O5 Nd3 O5 164.1(2) . 2 ?
O2 Nd3 O4 100.3(2) 1_565 2 ?
O2 Nd3 O4 73.5(2) 5_546 2 ?
O6 Nd3 O4 68.1(2) 5 2 ?
O6 Nd3 O4 118.5(2) . 2 ?
O5 Nd3 O4 116.61(18) . 2 ?
O5 Nd3 O4 64.55(18) 2 2 ?
O2 Nd3 O4 73.5(2) 1_565 . ?
O2 Nd3 O4 100.3(2) 5_546 . ?
O6 Nd3 O4 118.5(2) 5 . ?
O6 Nd3 O4 68.1(2) . . ?
O5 Nd3 O4 64.55(18) . . ?
O5 Nd3 O4 116.61(18) 2 . ?
O4 Nd3 O4 172.5(2) 2 . ?
O2 Nd3 Ta1 85.21(19) 1_565 2 ?
O2 Nd3 Ta1 95.98(19) 5_546 2 ?
O6 Nd3 Ta1 81.43(19) 5 2 ?
O6 Nd3 Ta1 97.38(19) . 2 ?
O5 Nd3 Ta1 146.64(12) . 2 ?
O5 Nd3 Ta1 32.98(12) 2 2 ?
O4 Nd3 Ta1 31.64(12) 2 2 ?
O4 Nd3 Ta1 148.54(12) . 2 ?
O2 Nd3 Ta1 95.98(19) 1_565 . ?
O2 Nd3 Ta1 85.21(19) 5_546 . ?
O6 Nd3 Ta1 97.38(19) 5 . ?
O6 Nd3 Ta1 81.43(19) . . ?
O5 Nd3 Ta1 32.98(12) . . ?
O5 Nd3 Ta1 146.64(12) 2 . ?
O4 Nd3 Ta1 148.54(12) 2 . ?
O4 Nd3 Ta1 31.64(12) . . ?
Ta1 Nd3 Ta1 178.517(19) 2 . ?
O2 Nd3 Nd3 37.36(15) 1_565 5_556 ?
O2 Nd3 Nd3 37.36(16) 5_546 5_556 ?
O6 Nd3 Nd3 142.63(14) 5 5_556 ?
O6 Nd3 Nd3 142.63(14) . 5_556 ?
O5 Nd3 Nd3 97.97(12) . 5_556 ?
O5 Nd3 Nd3 97.97(12) 2 5_556 ?
O4 Nd3 Nd3 86.24(11) 2 5_556 ?
O4 Nd3 Nd3 86.24(11) . 5_556 ?
Ta1 Nd3 Nd3 90.741(10) 2 5_556 ?
Ta1 Nd3 Nd3 90.741(10) . 5_556 ?
O2 Nd3 Nd2 35.14(18) 1_565 1_565 ?
O2 Nd3 Nd2 92.13(17) 5_546 1_565 ?
O6 Nd3 Nd2 154.62(16) 5 1_565 ?
O6 Nd3 Nd2 82.94(14) . 1_565 ?
O5 Nd3 Nd2 98.37(12) . 1_565 ?
O5 Nd3 Nd2 89.46(13) 2 1_565 ?
O4 Nd3 Nd2 135.14(11) 2 1_565 ?
O4 Nd3 Nd2 39.36(12) . 1_565 ?
Ta1 Nd3 Nd2 113.812(12) 2 1_565 ?
Ta1 Nd3 Nd2 66.981(11) . 1_565 ?
Nd3 Nd3 Nd2 60.588(9) 5_556 1_565 ?
O4 Ta1 O1 95.5(2) . . ?
O4 Ta1 O3 94.6(3) . . ?
O1 Ta1 O3 89.0(3) . . ?
O4 Ta1 O5 88.4(2) . . ?
O1 Ta1 O5 174.9(2) . . ?
O3 Ta1 O5 87.3(3) . . ?
O4 Ta1 O7 87.4(3) . . ?
O1 Ta1 O7 91.2(3) . . ?
O3 Ta1 O7 177.9(3) . . ?
O5 Ta1 O7 92.3(3) . . ?
O4 Ta1 O1 168.8(2) . 3_545 ?
O1 Ta1 O1 95.21(10) . 3_545 ?
O3 Ta1 O1 88.8(3) . 3_545 ?
O5 Ta1 O1 81.1(2) . 3_545 ?
O7 Ta1 O1 89.2(3) . 3_545 ?
O4 Ta1 Nd1 123.50(17) . 1_545 ?
O1 Ta1 Nd1 134.66(16) . 1_545 ?
O3 Ta1 Nd1 107.9(2) . 1_545 ?
O5 Ta1 Nd1 43.79(16) . 1_545 ?
O7 Ta1 Nd1 70.5(2) . 1_545 ?
O1 Ta1 Nd1 45.46(16) 3_545 1_545 ?
O4 Ta1 Nd2 100.53(16) . . ?
O1 Ta1 Nd2 129.68(16) . . ?
O3 Ta1 Nd2 42.6(2) . . ?
O5 Ta1 Nd2 45.96(16) . . ?
O7 Ta1 Nd2 136.5(2) . . ?
O1 Ta1 Nd2 74.93(15) 3_545 . ?
Nd1 Ta1 Nd2 69.597(11) 1_545 . ?
O4 Ta1 Nd1 45.45(15) . . ?
O1 Ta1 Nd1 83.97(16) . . ?
O3 Ta1 Nd1 138.1(2) . . ?
O5 Ta1 Nd1 101.15(16) . . ?
O7 Ta1 Nd1 44.0(2) . . ?
O1 Ta1 Nd1 132.94(15) 3_545 . ?
Nd1 Ta1 Nd1 106.211(10) 1_545 . ?
Nd2 Ta1 Nd1 138.287(17) . . ?
O4 Ta1 Nd3 45.17(17) . . ?
O1 Ta1 Nd3 140.17(16) . . ?
O3 Ta1 Nd3 88.8(2) . . ?
O5 Ta1 Nd3 43.37(16) . . ?
O7 Ta1 Nd3 92.3(2) . . ?
O1 Ta1 Nd3 124.48(16) 3_545 . ?
Nd1 Ta1 Nd3 83.360(14) 1_545 . ?
Nd2 Ta1 Nd3 66.586(13) . . ?
Nd1 Ta1 Nd3 71.702(13) . . ?
Ta1 O1 Ta1 141.3(3) . 3 ?
Ta1 O1 Nd1 120.3(2) . 3_545 ?
Ta1 O1 Nd1 98.4(2) 3 3_545 ?
Nd2 O2 Nd2 107.8(3) 5_546 . ?
Nd2 O2 Nd3 112.7(2) 5_546 1_545 ?
Nd2 O2 Nd3 109.2(2) . 1_545 ?
Nd2 O2 Nd3 112.7(2) 5_546 5_546 ?
Nd2 O2 Nd3 109.2(2) . 5_546 ?
Nd3 O2 Nd3 105.3(3) 1_545 5_546 ?
Ta1 O3 Ta1 147.6(4) . 6_556 ?
Ta1 O3 Nd2 103.7(2) . . ?
Ta1 O3 Nd2 103.7(2) 6_556 . ?
Ta1 O4 Nd2 137.9(3) . 1_565 ?
Ta1 O4 Nd1 102.0(2) . . ?
Nd2 O4 Nd1 105.9(2) 1_565 . ?
Ta1 O4 Nd3 103.2(2) . . ?
Nd2 O4 Nd3 98.02(19) 1_565 . ?
Nd1 O4 Nd3 107.04(19) . . ?
Ta1 O5 Nd1 102.0(2) . 1_545 ?
Ta1 O5 Nd3 103.6(2) . . ?
Nd1 O5 Nd3 140.3(2) 1_545 . ?
Ta1 O5 Nd2 99.7(2) . . ?
Nd1 O5 Nd2 105.2(2) 1_545 . ?
Nd3 O5 Nd2 99.8(2) . . ?
Nd1 O6 Nd3 114.5(2) . 5 ?
Nd1 O6 Nd3 114.5(2) . . ?
Nd3 O6 Nd3 105.3(3) 5 . ?
Ta1 O7 Ta1 151.0(4) 6 . ?
Ta1 O7 Nd1 101.9(2) 6 . ?
Ta1 O7 Nd1 101.9(2) . . ?

_refine_diff_density_max         1.398
_refine_diff_density_min         -1.380
_refine_diff_density_rms         0.344


# start Validation Reply Form
_vrf_PLAT430_5                   
;
PROBLEM: Short Inter D...A Contact  O2       ..O2       .       2.84 Ang.  
RESPONSE: This is not a D-H---A contact, and the distance reported in
this alert is simply an O---O interatomic distance.  The O2 atom has 
a satisfied bond valence sum, and does not support a hydrogen atom in
this dense structure.
;
# end Validation Reply Form
####################################################################### 
# 
# 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 1888861'
loop_
_audit_author_name
_audit_author_address
'Colin McMillen'
;Clemson University
United States of America
;
_audit_update_record             
;
2019-01-04 deposited with the CCDC.	2019-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'H La2 O6 Ta'
_chemical_formula_weight         555.78

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.0897(3)
_cell_length_b                   6.7199(4)
_cell_length_c                   10.2645(5)
_cell_angle_alpha                90
_cell_angle_beta                 94.158(2)
_cell_angle_gamma                90
_cell_volume                     487.73(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    6643
_cell_measurement_theta_min      3.03
_cell_measurement_theta_max      30.50

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    .
_exptl_crystal_density_diffrn    7.569
_exptl_crystal_F_000             944
_exptl_transmission_factor_min   .
_exptl_transmission_factor_max   .
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    39.526
_shelx_estimated_absorpt_T_min   0.144
_shelx_estimated_absorpt_T_max   0.200
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2900
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'SADABS, Bruker'
_exptl_absorpt_special_details   .
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   Ius
_diffrn_measurement_device_type  'Bruker Photon 100'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean .
_diffrn_reflns_number            9192
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.381
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1013
_reflns_number_gt                972
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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 APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT-2014 (Sheldrick 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND (Bradenburg, 1999)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0140P)²+2.6660P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.00421(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1013
_refine_ls_number_parameters     86
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0181
_refine_ls_R_factor_gt           0.0166
_refine_ls_wR_factor_ref         0.0370
_refine_ls_wR_factor_gt          0.0365
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_restrained_S_all      1.180
_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_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
La1 La -0.37481(5) 0.08891(6) 0.21182(3) 0.01995(11) Uani 1 1 d . . . . .
La2 La 0.11894(5) 0.22576(6) 0.08721(3) 0.01988(11) Uani 1 1 d . . . . .
Ta1 Ta 0.13749(3) 0.15066(4) 0.42698(2) 0.01698(10) Uani 1 1 d . . . . .
O1 O -0.0498(6) 0.1509(6) 0.5728(4) 0.0196(9) Uani 1 1 d . . . . .
O2 O 0.2988(6) 0.0781(7) 0.2913(4) 0.0191(9) Uani 1 1 d . . . . .
O3 O -0.0590(6) 0.2335(7) 0.2921(4) 0.0235(10) Uani 1 1 d . . . . .
O4 O 0.0779(6) 0.1138(6) -0.1415(4) 0.0166(8) Uani 1 1 d D . . . .
H4 H 0.051(9) -0.012(5) -0.169(6) 0.020 Uiso 1 1 d D U . . .
O5 O 0.3322(6) 0.0519(8) 0.5624(4) 0.0295(11) Uani 1 1 d . . . . .
O6 O 0.2015(9) 0.4149(8) 0.4724(5) 0.0430(15) 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
La1 O3 2.433(5) 2_445 ?
La1 O5 2.502(4) 3_556 ?
La1 O2 2.510(4) 1_455 ?
La1 O3 2.524(4) . ?
La1 O1 2.525(4) 4_565 ?
La1 O4 2.538(4) 4_566 ?
La1 O6 2.555(5) 4_565 ?
La1 O4 2.651(4) 3 ?
La1 Ta1 3.4139(5) 4_565 ?
La1 La2 3.7046(5) 2_445 ?
La1 Ta1 3.7130(5) 2_445 ?
La1 La2 3.8338(5) 1_455 ?
La1 H4 2.42(7) 3 ?
La2 O4 2.462(4) . ?
La2 O1 2.505(4) 4_665 ?
La2 O5 2.521(5) 4_565 ?
La2 O3 2.530(4) . ?
La2 O6 2.544(5) 2_545 ?
La2 O2 2.571(4) . ?
La2 O5 2.713(6) 2 ?
La2 O2 2.720(4) 2 ?
La2 O4 2.753(4) 3 ?
La2 Ta1 3.3455(5) 2 ?
La2 Ta1 3.5169(5) . ?
La2 H4 2.09(5) 3 ?
Ta1 O6 1.883(5) . ?
Ta1 O2 1.928(4) . ?
Ta1 O3 1.972(4) . ?
Ta1 O5 2.000(4) . ?
Ta1 O1 2.072(4) . ?
Ta1 O1 2.120(4) 3_556 ?
Ta1 Ta1 3.2513(5) 3_556 ?
O4 H4 0.91(2) . ?

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
O3 La1 O5 69.78(16) 2_445 3_556 ?
O3 La1 O2 78.22(14) 2_445 1_455 ?
O5 La1 O2 74.94(14) 3_556 1_455 ?
O3 La1 O3 123.28(14) 2_445 . ?
O5 La1 O3 78.37(14) 3_556 . ?
O2 La1 O3 136.21(14) 1_455 . ?
O3 La1 O1 125.73(14) 2_445 4_565 ?
O5 La1 O1 143.80(15) 3_556 4_565 ?
O2 La1 O1 77.11(14) 1_455 4_565 ?
O3 La1 O1 107.80(14) . 4_565 ?
O3 La1 O4 138.47(14) 2_445 4_566 ?
O5 La1 O4 76.14(16) 3_556 4_566 ?
O2 La1 O4 70.44(13) 1_455 4_566 ?
O3 La1 O4 69.85(14) . 4_566 ?
O1 La1 O4 73.10(13) 4_565 4_566 ?
O3 La1 O6 91.62(17) 2_445 4_565 ?
O5 La1 O6 150.21(17) 3_556 4_565 ?
O2 La1 O6 125.24(18) 1_455 4_565 ?
O3 La1 O6 94.21(18) . 4_565 ?
O1 La1 O6 65.98(15) 4_565 4_565 ?
O4 La1 O6 128.66(15) 4_566 4_565 ?
O3 La1 O4 69.34(14) 2_445 3 ?
O5 La1 O4 90.74(15) 3_556 3 ?
O2 La1 O4 147.43(14) 1_455 3 ?
O3 La1 O4 65.39(14) . 3 ?
O1 La1 O4 124.70(13) 4_565 3 ?
O4 La1 O4 135.03(8) 4_566 3 ?
O6 La1 O4 60.35(15) 4_565 3 ?
O3 La1 Ta1 120.37(10) 2_445 4_565 ?
O5 La1 Ta1 168.12(11) 3_556 4_565 ?
O2 La1 Ta1 112.00(10) 1_455 4_565 ?
O3 La1 Ta1 90.30(10) . 4_565 ?
O1 La1 Ta1 37.17(10) 4_565 4_565 ?
O4 La1 Ta1 96.73(9) 4_566 4_565 ?
O6 La1 Ta1 32.95(11) 4_565 4_565 ?
O4 La1 Ta1 87.72(9) 3 4_565 ?
O3 La1 La2 42.74(10) 2_445 2_445 ?
O5 La1 La2 42.67(11) 3_556 2_445 ?
O2 La1 La2 47.24(10) 1_455 2_445 ?
O3 La1 La2 120.73(10) . 2_445 ?
O1 La1 La2 122.73(10) 4_565 2_445 ?
O4 La1 La2 95.80(9) 4_566 2_445 ?
O6 La1 La2 132.01(14) 4_565 2_445 ?
O4 La1 La2 103.02(10) 3 2_445 ?
Ta1 La1 La2 148.928(13) 4_565 2_445 ?
O3 La1 Ta1 28.90(10) 2_445 2_445 ?
O5 La1 Ta1 94.53(12) 3_556 2_445 ?
O2 La1 Ta1 69.71(10) 1_455 2_445 ?
O3 La1 Ta1 147.05(11) . 2_445 ?
O1 La1 Ta1 96.91(10) 4_565 2_445 ?
O4 La1 Ta1 140.14(9) 4_566 2_445 ?
O6 La1 Ta1 76.01(14) 4_565 2_445 ?
O4 La1 Ta1 82.77(9) 3 2_445 ?
Ta1 La1 Ta1 96.962(11) 4_565 2_445 ?
La2 La1 Ta1 56.606(9) 2_445 2_445 ?
O3 La1 La2 93.16(10) 2_445 1_455 ?
O5 La1 La2 116.56(10) 3_556 1_455 ?
O2 La1 La2 41.62(10) 1_455 1_455 ?
O3 La1 La2 143.47(11) . 1_455 ?
O1 La1 La2 40.16(10) 4_565 1_455 ?
O4 La1 La2 81.27(9) 4_566 1_455 ?
O6 La1 La2 86.55(14) 4_565 1_455 ?
O4 La1 La2 140.81(9) 3 1_455 ?
Ta1 La1 La2 70.899(10) 4_565 1_455 ?
La2 La1 La2 83.102(10) 2_445 1_455 ?
Ta1 La1 La2 68.337(9) 2_445 1_455 ?
O3 La1 H4 88.4(7) 2_445 3 ?
O5 La1 H4 92.0(16) 3_556 3 ?
O2 La1 H4 163.8(13) 1_455 3 ?
O3 La1 H4 46.5(8) . 3 ?
O1 La1 H4 118.5(15) 4_565 3 ?
O4 La1 H4 116.3(7) 4_566 3 ?
O6 La1 H4 63.5(16) 4_565 3 ?
O4 La1 H4 19.9(5) 3 3 ?
Ta1 La1 H4 82.5(16) 4_565 3 ?
La2 La1 H4 116.6(13) 2_445 3 ?
Ta1 La1 H4 102.5(6) 2_445 3 ?
La2 La1 H4 150.0(16) 1_455 3 ?
O4 La2 O1 95.25(14) . 4_665 ?
O4 La2 O5 92.63(14) . 4_565 ?
O1 La2 O5 123.41(16) 4_665 4_565 ?
O4 La2 O3 140.11(14) . . ?
O1 La2 O3 124.62(14) 4_665 . ?
O5 La2 O3 67.97(15) 4_565 . ?
O4 La2 O6 63.04(16) . 2_545 ?
O1 La2 O6 76.70(18) 4_665 2_545 ?
O5 La2 O6 151.19(19) 4_565 2_545 ?
O3 La2 O6 120.33(16) . 2_545 ?
O4 La2 O2 132.55(14) . . ?
O1 La2 O2 76.34(13) 4_665 . ?
O5 La2 O2 131.29(14) 4_565 . ?
O3 La2 O2 65.07(13) . . ?
O6 La2 O2 69.62(16) 2_545 . ?
O4 La2 O5 73.65(14) . 2 ?
O1 La2 O5 62.65(13) 4_665 2 ?
O5 La2 O5 66.36(17) 4_565 2 ?
O3 La2 O5 123.06(14) . 2 ?
O6 La2 O5 116.16(15) 2_545 2 ?
O2 La2 O5 134.16(13) . 2 ?
O4 La2 O2 135.22(14) . 2 ?
O1 La2 O2 64.41(13) 4_665 2 ?
O5 La2 O2 71.03(15) 4_565 2 ?
O3 La2 O2 72.79(14) . 2 ?
O6 La2 O2 136.96(18) 2_545 2 ?
O2 La2 O2 83.41(6) . 2 ?
O5 La2 O2 61.58(13) 2 2 ?
O4 La2 O4 85.02(14) . 3 ?
O1 La2 O4 141.02(13) 4_665 3 ?
O5 La2 O4 95.44(15) 4_565 3 ?
O3 La2 O4 63.78(14) . 3 ?
O6 La2 O4 68.76(16) 2_545 3 ?
O2 La2 O4 75.17(13) . 3 ?
O5 La2 O4 150.67(13) 2 3 ?
O2 La2 O4 136.38(12) 2 3 ?
O4 La2 Ta1 104.18(10) . 2 ?
O1 La2 Ta1 39.28(10) 4_665 2 ?
O5 La2 Ta1 84.54(12) 4_565 2 ?
O3 La2 Ta1 107.97(11) . 2 ?
O6 La2 Ta1 114.93(15) 2_545 2 ?
O2 La2 Ta1 97.91(10) . 2 ?
O5 La2 Ta1 36.70(9) 2 2 ?
O2 La2 Ta1 35.19(9) 2 2 ?
O4 La2 Ta1 170.80(9) 3 2 ?
O4 La2 Ta1 153.50(10) . . ?
O1 La2 Ta1 97.94(10) 4_665 . ?
O5 La2 Ta1 99.05(10) 4_565 . ?
O3 La2 Ta1 33.25(10) . . ?
O6 La2 Ta1 97.88(12) 2_545 . ?
O2 La2 Ta1 32.44(9) . . ?
O5 La2 Ta1 132.85(10) 2 . ?
O2 La2 Ta1 71.27(9) 2 . ?
O4 La2 Ta1 70.33(8) 3 . ?
Ta1 La2 Ta1 100.566(11) 2 . ?
O4 La2 La1 134.79(9) . 2_455 ?
O1 La2 La1 107.02(10) 4_665 2_455 ?
O5 La2 La1 42.28(10) 4_565 2_455 ?
O3 La2 La1 40.74(11) . 2_455 ?
O6 La2 La1 159.54(11) 2_545 2_455 ?
O2 La2 La1 91.41(9) . 2_455 ?
O5 La2 La1 82.35(10) 2 2_455 ?
O2 La2 La1 42.65(9) 2 2_455 ?
O4 La2 La1 99.74(8) 3 2_455 ?
Ta1 La2 La1 74.070(11) 2 2_455 ?
Ta1 La2 La1 61.817(10) . 2_455 ?
O4 La2 H4 98.1(14) . 3 ?
O1 La2 H4 145.3(19) 4_665 3 ?
O5 La2 H4 87.9(17) 4_565 3 ?
O3 La2 H4 49.0(13) . 3 ?
O6 La2 H4 81.1(14) 2_545 3 ?
O2 La2 H4 71.0(18) . 3 ?
O5 La2 H4 152.1(19) 2 3 ?
O2 La2 H4 121.7(13) 2 3 ?
O4 La2 H4 14.8(13) 3 3 ?
Ta1 La2 H4 156.8(13) 2 3 ?
Ta1 La2 H4 59.0(16) . 3 ?
La1 La2 H4 85.6(13) 2_455 3 ?
O6 Ta1 O2 105.8(2) . . ?
O6 Ta1 O3 93.0(2) . . ?
O2 Ta1 O3 89.44(18) . . ?
O6 Ta1 O5 89.9(3) . . ?
O2 Ta1 O5 90.13(19) . . ?
O3 Ta1 O5 177.0(2) . . ?
O6 Ta1 O1 88.6(2) . . ?
O2 Ta1 O1 165.26(18) . . ?
O3 Ta1 O1 92.87(18) . . ?
O5 Ta1 O1 86.80(18) . . ?
O6 Ta1 O1 165.20(19) . 3_556 ?
O2 Ta1 O1 87.05(18) . 3_556 ?
O3 Ta1 O1 94.48(18) . 3_556 ?
O5 Ta1 O1 82.54(19) . 3_556 ?
O1 Ta1 O1 78.26(18) . 3_556 ?
O6 Ta1 Ta1 127.96(15) . 3_556 ?
O2 Ta1 Ta1 125.64(13) . 3_556 ?
O3 Ta1 Ta1 94.75(13) . 3_556 ?
O5 Ta1 Ta1 83.10(14) . 3_556 ?
O1 Ta1 Ta1 39.66(12) . 3_556 ?
O1 Ta1 Ta1 38.60(11) 3_556 3_556 ?
O6 Ta1 La2 134.4(2) . 2_545 ?
O2 Ta1 La2 54.38(13) . 2_545 ?
O3 Ta1 La2 123.45(14) . 2_545 ?
O5 Ta1 La2 54.17(16) . 2_545 ?
O1 Ta1 La2 113.07(12) . 2_545 ?
O1 Ta1 La2 48.44(12) 3_556 2_545 ?
Ta1 Ta1 La2 79.467(12) 3_556 2_545 ?
O6 Ta1 La1 47.58(15) . 4_666 ?
O2 Ta1 La1 143.28(13) . 4_666 ?
O3 Ta1 La1 113.32(14) . 4_666 ?
O5 Ta1 La1 68.54(15) . 4_666 ?
O1 Ta1 La1 47.41(12) . 4_666 ?
O1 Ta1 La1 117.62(11) 3_556 4_666 ?
Ta1 Ta1 La1 82.591(11) 3_556 4_666 ?
La2 Ta1 La1 121.339(11) 2_545 4_666 ?
O6 Ta1 La2 95.80(16) . . ?
O2 Ta1 La2 45.68(13) . . ?
O3 Ta1 La2 44.73(13) . . ?
O5 Ta1 La2 135.32(13) . . ?
O1 Ta1 La2 137.45(12) . . ?
O1 Ta1 La2 98.52(11) 3_556 . ?
Ta1 Ta1 La2 124.471(13) 3_556 . ?
La2 Ta1 La2 93.531(10) 2_545 . ?
La1 Ta1 La2 140.737(12) 4_666 . ?
O6 Ta1 La1 56.8(2) . 2_455 ?
O2 Ta1 La1 103.33(13) . 2_455 ?
O3 Ta1 La1 36.62(14) . 2_455 ?
O5 Ta1 La1 146.26(16) . 2_455 ?
O1 Ta1 La1 86.96(12) . 2_455 ?
O1 Ta1 La1 128.28(12) 3_556 2_455 ?
Ta1 Ta1 La1 111.719(12) 3_556 2_455 ?
La2 Ta1 La1 155.005(11) 2_545 2_455 ?
La1 Ta1 La1 83.037(11) 4_666 2_455 ?
La2 Ta1 La1 61.577(9) . 2_455 ?
O6 Ta1 La2 59.4(2) . 4_666 ?
O2 Ta1 La2 78.76(12) . 4_666 ?
O3 Ta1 La2 144.57(14) . 4_666 ?
O5 Ta1 La2 38.08(15) . 4_666 ?
O1 Ta1 La2 106.96(12) . 4_666 ?
O1 Ta1 La2 117.80(12) 3_556 4_666 ?
Ta1 Ta1 La2 119.335(12) 3_556 4_666 ?
La2 Ta1 La2 75.716(11) 2_545 4_666 ?
La1 Ta1 La2 65.938(9) 4_666 4_666 ?
La2 Ta1 La2 111.613(11) . 4_666 ?
La1 Ta1 La2 113.921(10) 2_455 4_666 ?
Ta1 O1 Ta1 101.74(18) . 3_556 ?
Ta1 O1 La2 134.1(2) . 4_566 ?
Ta1 O1 La2 92.28(15) 3_556 4_566 ?
Ta1 O1 La1 95.42(16) . 4_666 ?
Ta1 O1 La1 142.5(2) 3_556 4_666 ?
La2 O1 La1 99.31(15) 4_566 4_666 ?
Ta1 O2 La1 146.8(2) . 1_655 ?
Ta1 O2 La2 101.88(17) . . ?
La1 O2 La2 97.96(14) 1_655 . ?
Ta1 O2 La2 90.43(16) . 2_545 ?
La1 O2 La2 90.12(13) 1_655 2_545 ?
La2 O2 La2 141.87(18) . 2_545 ?
Ta1 O3 La1 114.5(2) . 2_455 ?
Ta1 O3 La1 133.3(2) . . ?
La1 O3 La1 101.95(16) 2_455 . ?
Ta1 O3 La2 102.02(18) . . ?
La1 O3 La2 96.52(16) 2_455 . ?
La1 O3 La2 101.80(16) . . ?
La2 O4 La1 108.27(15) . 4_665 ?
La2 O4 La1 112.04(15) . 3 ?
La1 O4 La1 95.81(14) 4_665 3 ?
La2 O4 La2 94.98(14) . 3 ?
La1 O4 La2 149.68(16) 4_665 3 ?
La1 O4 La2 93.06(13) 3 3 ?
La2 O4 H4 126(4) . . ?
La1 O4 H4 126(4) 4_665 . ?
La1 O4 H4 66(4) 3 . ?
La2 O4 H4 36(4) 3 . ?
Ta1 O5 La1 143.2(2) . 3_556 ?
Ta1 O5 La2 112.6(2) . 4_666 ?
La1 O5 La2 95.05(15) 3_556 4_666 ?
Ta1 O5 La2 89.13(17) . 2_545 ?
La1 O5 La2 101.94(19) 3_556 2_545 ?
La2 O5 La2 113.64(17) 4_666 2_545 ?
Ta1 O6 La2 146.2(3) . 2 ?
Ta1 O6 La1 99.5(2) . 4_666 ?
La2 O6 La1 112.58(19) 2 4_666 ?

_refine_diff_density_max         0.814
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.201

####################################################################### 
# 
# 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 1888862'
loop_
_audit_author_name
_audit_author_address
'Colin McMillen'
;Clemson University
United States of America
;
_audit_update_record             
;
2019-01-04 deposited with the CCDC.	2019-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'H O6 Pr2 Ta'
_chemical_formula_weight         559.78

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.0137(3)
_cell_length_b                   6.7134(3)
_cell_length_c                   10.1240(4)
_cell_angle_alpha                90
_cell_angle_beta                 94.122(2)
_cell_angle_gamma                90
_cell_volume                     475.46(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    299(2)
_cell_measurement_reflns_used    5289
_cell_measurement_theta_min      3.42
_cell_measurement_theta_max      30.63

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    .
_exptl_crystal_density_diffrn    7.820
_exptl_crystal_F_000             960
_exptl_transmission_factor_min   .
_exptl_transmission_factor_max   .
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    43.070
_shelx_estimated_absorpt_T_min   0.130
_shelx_estimated_absorpt_T_max   0.182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3510
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'SADABS, Bruker'
_exptl_absorpt_special_details   .
_diffrn_ambient_temperature      299(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   Ius
_diffrn_measurement_device_type  'Bruker Photon 100'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean .
_diffrn_reflns_number            5479
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.422
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             887
_reflns_number_gt                859
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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 APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT-2014 (Sheldrick 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND (Bradenburg, 1999)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0136P)²+1.9928P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.0225(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         887
_refine_ls_number_parameters     86
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0169
_refine_ls_R_factor_gt           0.0160
_refine_ls_wR_factor_ref         0.0389
_refine_ls_wR_factor_gt          0.0384
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_restrained_S_all      1.118
_refine_ls_shift/su_max          0.000
_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_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
Pr1 Pr -0.36844(5) 0.07984(5) 0.21155(3) 0.00939(13) Uani 1 1 d . . . . .
Pr2 Pr 0.11888(5) 0.23184(5) 0.08268(3) 0.01007(13) Uani 1 1 d . . . . .
Ta1 Ta 0.13601(4) 0.15359(4) 0.42723(2) 0.00769(12) Uani 1 1 d . . . . .
O1 O -0.0492(7) 0.1518(6) 0.5749(4) 0.0103(10) Uani 1 1 d . . . . .
O2 O 0.2960(7) 0.0798(6) 0.2864(4) 0.0102(9) Uani 1 1 d . . . . .
O3 O -0.0637(7) 0.2348(7) 0.2903(5) 0.0125(10) Uani 1 1 d . . . . .
O4 O 0.0702(7) 0.1140(7) -0.1438(5) 0.0142(10) Uani 1 1 d D . . . .
H4 H -0.041(7) 0.129(12) -0.197(6) 0.020 Uiso 1 1 d D U . . .
O5 O 0.3355(7) 0.0514(7) 0.5618(4) 0.0130(10) Uani 1 1 d . . . . .
O6 O 0.1980(8) 0.4195(7) 0.4723(5) 0.0191(11) 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
Pr1 O3 2.365(4) 2_445 ?
Pr1 O5 2.453(4) 3_556 ?
Pr1 O3 2.458(5) . ?
Pr1 O6 2.500(5) 4_565 ?
Pr1 O2 2.524(4) 1_455 ?
Pr1 O1 2.552(4) 4_565 ?
Pr1 O4 2.577(5) 4_566 ?
Pr1 O4 2.598(5) 3 ?
Pr1 Ta1 3.3914(4) 4_565 ?
Pr1 Ta1 3.6476(4) 2_445 ?
Pr1 Pr2 3.6619(5) 2_445 ?
Pr1 Pr1 3.8011(4) 2_455 ?
Pr2 O4 2.427(5) . ?
Pr2 O5 2.460(5) 4_565 ?
Pr2 O1 2.463(5) 4_665 ?
Pr2 O3 2.539(5) . ?
Pr2 O6 2.541(5) 2_545 ?
Pr2 O2 2.544(5) . ?
Pr2 O5 2.629(5) 2 ?
Pr2 O2 2.731(4) 2 ?
Pr2 O4 2.766(5) 3 ?
Pr2 Ta1 3.3177(5) 2 ?
Pr2 Ta1 3.5211(5) . ?
Ta1 O6 1.886(5) . ?
Ta1 O2 1.941(4) . ?
Ta1 O3 1.975(5) . ?
Ta1 O5 2.003(5) . ?
Ta1 O1 2.050(4) . ?
Ta1 O1 2.138(4) 3_556 ?
Ta1 Ta1 3.2354(5) 3_556 ?
O4 H4 0.92(2) . ?

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
O3 Pr1 O5 70.17(16) 2_445 3_556 ?
O3 Pr1 O3 125.93(14) 2_445 . ?
O5 Pr1 O3 80.06(15) 3_556 . ?
O3 Pr1 O6 92.60(16) 2_445 4_565 ?
O5 Pr1 O6 153.57(16) 3_556 4_565 ?
O3 Pr1 O6 95.47(17) . 4_565 ?
O3 Pr1 O2 79.10(15) 2_445 1_455 ?
O5 Pr1 O2 75.30(15) 3_556 1_455 ?
O3 Pr1 O2 135.29(14) . 1_455 ?
O6 Pr1 O2 122.26(16) 4_565 1_455 ?
O3 Pr1 O1 126.56(15) 2_445 4_565 ?
O5 Pr1 O1 140.36(15) 3_556 4_565 ?
O3 Pr1 O1 105.27(15) . 4_565 ?
O6 Pr1 O1 66.02(15) 4_565 4_565 ?
O2 Pr1 O1 74.05(14) 1_455 4_565 ?
O3 Pr1 O4 138.06(15) 2_445 4_566 ?
O5 Pr1 O4 76.32(16) 3_556 4_566 ?
O3 Pr1 O4 69.83(15) . 4_566 ?
O6 Pr1 O4 126.84(15) 4_565 4_566 ?
O2 Pr1 O4 68.41(15) 1_455 4_566 ?
O1 Pr1 O4 69.40(15) 4_565 4_566 ?
O3 Pr1 O4 70.88(16) 2_445 3 ?
O5 Pr1 O4 92.49(15) 3_556 3 ?
O3 Pr1 O4 66.39(15) . 3 ?
O6 Pr1 O4 62.31(16) 4_565 3 ?
O2 Pr1 O4 149.92(14) 1_455 3 ?
O1 Pr1 O4 126.07(15) 4_565 3 ?
O4 Pr1 O4 136.06(10) 4_566 3 ?
O3 Pr1 Ta1 121.63(11) 2_445 4_565 ?
O5 Pr1 Ta1 167.78(11) 3_556 4_565 ?
O3 Pr1 Ta1 89.49(11) . 4_565 ?
O6 Pr1 Ta1 33.16(11) 4_565 4_565 ?
O2 Pr1 Ta1 108.69(10) 1_455 4_565 ?
O1 Pr1 Ta1 37.07(10) 4_565 4_565 ?
O4 Pr1 Ta1 94.21(10) 4_566 4_565 ?
O4 Pr1 Ta1 89.07(11) 3 4_565 ?
O3 Pr1 Ta1 29.64(12) 2_445 2_445 ?
O5 Pr1 Ta1 95.15(11) 3_556 2_445 ?
O3 Pr1 Ta1 150.26(11) . 2_445 ?
O6 Pr1 Ta1 75.79(12) 4_565 2_445 ?
O2 Pr1 Ta1 69.54(10) 1_455 2_445 ?
O1 Pr1 Ta1 97.09(10) 4_565 2_445 ?
O4 Pr1 Ta1 137.90(11) 4_566 2_445 ?
O4 Pr1 Ta1 84.67(10) 3 2_445 ?
Ta1 Pr1 Ta1 97.061(11) 4_565 2_445 ?
O3 Pr1 Pr2 43.53(11) 2_445 2_445 ?
O5 Pr1 Pr2 41.88(11) 3_556 2_445 ?
O3 Pr1 Pr2 121.80(11) . 2_445 ?
O6 Pr1 Pr2 133.07(12) 4_565 2_445 ?
O2 Pr1 Pr2 48.19(10) 1_455 2_445 ?
O1 Pr1 Pr2 121.26(10) 4_565 2_445 ?
O4 Pr1 Pr2 94.53(11) 4_566 2_445 ?
O4 Pr1 Pr2 105.00(11) 3 2_445 ?
Ta1 Pr1 Pr2 148.602(13) 4_565 2_445 ?
Ta1 Pr1 Pr2 57.595(9) 2_445 2_445 ?
O3 Pr1 Pr1 162.07(12) 2_445 2_455 ?
O5 Pr1 Pr1 96.62(11) 3_556 2_455 ?
O3 Pr1 Pr1 37.13(10) . 2_455 ?
O6 Pr1 Pr1 95.04(12) 4_565 2_455 ?
O2 Pr1 Pr1 110.00(10) 1_455 2_455 ?
O1 Pr1 Pr1 71.35(10) 4_565 2_455 ?
O4 Pr1 Pr1 42.94(11) 4_566 2_455 ?
O4 Pr1 Pr1 98.52(11) 3 2_455 ?
Ta1 Pr1 Pr1 71.174(10) 4_565 2_455 ?
Ta1 Pr1 Pr1 167.658(16) 2_445 2_455 ?
Pr2 Pr1 Pr1 131.862(16) 2_445 2_455 ?
O4 Pr2 O5 93.07(15) . 4_565 ?
O4 Pr2 O1 98.20(16) . 4_665 ?
O5 Pr2 O1 124.71(15) 4_565 4_665 ?
O4 Pr2 O3 137.71(16) . . ?
O5 Pr2 O3 67.29(14) 4_565 . ?
O1 Pr2 O3 123.94(15) 4_665 . ?
O4 Pr2 O6 64.11(16) . 2_545 ?
O5 Pr2 O6 152.53(16) 4_565 2_545 ?
O1 Pr2 O6 76.17(16) 4_665 2_545 ?
O3 Pr2 O6 118.72(15) . 2_545 ?
O4 Pr2 O2 131.52(15) . . ?
O5 Pr2 O2 130.65(14) 4_565 . ?
O1 Pr2 O2 75.25(14) 4_665 . ?
O3 Pr2 O2 65.03(14) . . ?
O6 Pr2 O2 67.74(15) 2_545 . ?
O4 Pr2 O5 75.79(15) . 2 ?
O5 Pr2 O5 66.38(18) 4_565 2 ?
O1 Pr2 O5 64.55(14) 4_665 2 ?
O3 Pr2 O5 122.90(14) . 2 ?
O6 Pr2 O5 117.90(15) 2_545 2 ?
O2 Pr2 O5 134.97(14) . 2 ?
O4 Pr2 O2 138.47(15) . 2 ?
O5 Pr2 O2 71.51(15) 4_565 2 ?
O1 Pr2 O2 64.51(14) 4_665 2 ?
O3 Pr2 O2 72.38(14) . 2 ?
O6 Pr2 O2 135.70(16) 2_545 2 ?
O2 Pr2 O2 82.68(6) . 2 ?
O5 Pr2 O2 62.68(14) 2 2 ?
O4 Pr2 O4 84.31(16) . 3 ?
O5 Pr2 O4 96.81(15) 4_565 3 ?
O1 Pr2 O4 137.99(14) 4_665 3 ?
O3 Pr2 O4 62.79(14) . 3 ?
O6 Pr2 O4 67.31(16) 2_545 3 ?
O2 Pr2 O4 72.28(14) . 3 ?
O5 Pr2 O4 152.75(14) 2 3 ?
O2 Pr2 O4 134.51(13) 2 3 ?
O4 Pr2 Ta1 106.72(12) . 2 ?
O5 Pr2 Ta1 84.82(12) 4_565 2 ?
O1 Pr2 Ta1 40.10(10) 4_665 2 ?
O3 Pr2 Ta1 108.17(10) . 2 ?
O6 Pr2 Ta1 115.24(12) 2_545 2 ?
O2 Pr2 Ta1 98.23(10) . 2 ?
O5 Pr2 Ta1 37.13(10) 2 2 ?
O2 Pr2 Ta1 35.80(9) 2 2 ?
O4 Pr2 Ta1 168.80(10) 3 2 ?
O4 Pr2 Ta1 151.65(11) . . ?
O5 Pr2 Ta1 98.23(10) 4_565 . ?
O1 Pr2 Ta1 96.54(11) 4_665 . ?
O3 Pr2 Ta1 33.31(11) . . ?
O6 Pr2 Ta1 96.43(11) 2_545 . ?
O2 Pr2 Ta1 32.54(10) . . ?
O5 Pr2 Ta1 132.54(10) 2 . ?
O2 Pr2 Ta1 69.88(9) 2 . ?
O4 Pr2 Ta1 68.64(10) 3 . ?
Ta1 Pr2 Ta1 100.161(11) 2 . ?
O4 Pr2 Pr1 134.82(11) . 2_455 ?
O5 Pr2 Pr1 41.74(10) 4_565 2_455 ?
O1 Pr2 Pr1 107.99(10) 4_665 2_455 ?
O3 Pr2 Pr1 39.91(10) . 2_455 ?
O6 Pr2 Pr1 157.15(11) 2_545 2_455 ?
O2 Pr2 Pr1 91.20(10) . 2_455 ?
O5 Pr2 Pr1 83.02(10) 2 2_455 ?
O2 Pr2 Pr1 43.54(9) 2 2_455 ?
O4 Pr2 Pr1 98.68(10) 3 2_455 ?
Ta1 Pr2 Pr1 75.138(10) 2 2_455 ?
Ta1 Pr2 Pr1 60.999(9) . 2_455 ?
O6 Ta1 O2 106.49(19) . . ?
O6 Ta1 O3 92.8(2) . . ?
O2 Ta1 O3 88.45(19) . . ?
O6 Ta1 O5 91.3(2) . . ?
O2 Ta1 O5 89.99(19) . . ?
O3 Ta1 O5 175.95(19) . . ?
O6 Ta1 O1 88.65(19) . . ?
O2 Ta1 O1 164.65(17) . . ?
O3 Ta1 O1 93.4(2) . . ?
O5 Ta1 O1 87.13(18) . . ?
O6 Ta1 O1 166.11(18) . 3_556 ?
O2 Ta1 O1 85.81(18) . 3_556 ?
O3 Ta1 O1 94.02(18) . 3_556 ?
O5 Ta1 O1 82.14(19) . 3_556 ?
O1 Ta1 O1 78.86(18) . 3_556 ?
O6 Ta1 Ta1 128.80(14) . 3_556 ?
O2 Ta1 Ta1 124.25(13) . 3_556 ?
O3 Ta1 Ta1 94.81(13) . 3_556 ?
O5 Ta1 Ta1 82.98(13) . 3_556 ?
O1 Ta1 Ta1 40.42(12) . 3_556 ?
O1 Ta1 Ta1 38.44(12) 3_556 3_556 ?
O6 Ta1 Pr2 134.78(17) . 2_545 ?
O2 Ta1 Pr2 55.38(13) . 2_545 ?
O3 Ta1 Pr2 123.85(13) . 2_545 ?
O5 Ta1 Pr2 52.41(14) . 2_545 ?
O1 Ta1 Pr2 111.95(12) . 2_545 ?
O1 Ta1 Pr2 47.88(13) 3_556 2_545 ?
Ta1 Ta1 Pr2 78.088(11) 3_556 2_545 ?
O6 Ta1 Pr1 46.47(14) . 4_666 ?
O2 Ta1 Pr1 143.06(14) . 4_666 ?
O3 Ta1 Pr1 113.63(13) . 4_666 ?
O5 Ta1 Pr1 69.63(14) . 4_666 ?
O1 Ta1 Pr1 48.63(12) . 4_666 ?
O1 Ta1 Pr1 119.65(12) 3_556 4_666 ?
Ta1 Ta1 Pr1 84.728(11) 3_556 4_666 ?
Pr2 Ta1 Pr1 120.822(12) 2_545 4_666 ?
O6 Ta1 Pr2 95.11(15) . . ?
O2 Ta1 Pr2 44.82(14) . . ?
O3 Ta1 Pr2 44.89(13) . . ?
O5 Ta1 Pr2 134.23(13) . . ?
O1 Ta1 Pr2 138.19(14) . . ?
O1 Ta1 Pr2 98.25(12) 3_556 . ?
Ta1 Ta1 Pr2 124.542(13) 3_556 . ?
Pr2 Ta1 Pr2 94.488(10) 2_545 . ?
Pr1 Ta1 Pr2 139.496(12) 4_666 . ?
O6 Ta1 Pr1 56.88(17) . 2_455 ?
O2 Ta1 Pr1 103.05(13) . 2_455 ?
O3 Ta1 Pr1 36.30(13) . 2_455 ?
O5 Ta1 Pr1 147.75(14) . 2_455 ?
O1 Ta1 Pr1 87.15(13) . 2_455 ?
O1 Ta1 Pr1 127.58(13) 3_556 2_455 ?
Ta1 Ta1 Pr1 111.812(13) 3_556 2_455 ?
Pr2 Ta1 Pr1 155.676(12) 2_545 2_455 ?
Pr1 Ta1 Pr1 82.939(11) 4_666 2_455 ?
Pr2 Ta1 Pr1 61.406(9) . 2_455 ?
O6 Ta1 Pr2 60.90(17) . 4_666 ?
O2 Ta1 Pr2 78.84(14) . 4_666 ?
O3 Ta1 Pr2 145.08(13) . 4_666 ?
O5 Ta1 Pr2 37.89(13) . 4_666 ?
O1 Ta1 Pr2 107.37(13) . 4_666 ?
O1 Ta1 Pr2 116.98(13) 3_556 4_666 ?
Ta1 Ta1 Pr2 119.276(13) 3_556 4_666 ?
Pr2 Ta1 Pr2 74.371(11) 2_545 4_666 ?
Pr1 Ta1 Pr2 66.079(9) 4_666 4_666 ?
Pr2 Ta1 Pr2 110.751(11) . 4_666 ?
Pr1 Ta1 Pr2 115.424(11) 2_455 4_666 ?
Ta1 O1 Ta1 101.14(18) . 3_556 ?
Ta1 O1 Pr2 132.2(2) . 4_566 ?
Ta1 O1 Pr2 92.02(17) 3_556 4_566 ?
Ta1 O1 Pr1 94.31(17) . 4_666 ?
Ta1 O1 Pr1 144.3(2) 3_556 4_666 ?
Pr2 O1 Pr1 101.10(15) 4_566 4_666 ?
Ta1 O2 Pr1 145.2(2) . 1_655 ?
Ta1 O2 Pr2 102.64(19) . . ?
Pr1 O2 Pr2 99.68(15) 1_655 . ?
Ta1 O2 Pr2 88.83(16) . 2_545 ?
Pr1 O2 Pr2 88.26(14) 1_655 2_545 ?
Pr2 O2 Pr2 144.48(19) . 2_545 ?
Ta1 O3 Pr1 114.1(2) . 2_455 ?
Ta1 O3 Pr1 131.9(2) . . ?
Pr1 O3 Pr1 104.02(17) 2_455 . ?
Ta1 O3 Pr2 101.79(19) . . ?
Pr1 O3 Pr2 96.56(16) 2_455 . ?
Pr1 O3 Pr2 101.94(17) . . ?
Pr2 O4 Pr1 105.01(17) . 4_665 ?
Pr2 O4 Pr1 110.57(18) . 3 ?
Pr1 O4 Pr1 94.53(16) 4_665 3 ?
Pr2 O4 Pr2 95.69(16) . 3 ?
Pr1 O4 Pr2 154.0(2) 4_665 3 ?
Pr1 O4 Pr2 92.67(15) 3 3 ?
Pr2 O4 H4 125(5) . . ?
Pr1 O4 H4 75(5) 4_665 . ?
Pr1 O4 H4 124(5) 3 . ?
Pr2 O4 H4 80(5) 3 . ?
Ta1 O5 Pr1 140.7(2) . 3_556 ?
Ta1 O5 Pr2 112.1(2) . 4_666 ?
Pr1 O5 Pr2 96.37(16) 3_556 4_666 ?
Ta1 O5 Pr2 90.46(16) . 2_545 ?
Pr1 O5 Pr2 102.73(17) 3_556 2_545 ?
Pr2 O5 Pr2 113.62(18) 4_666 2_545 ?
Ta1 O6 Pr1 100.37(19) . 4_666 ?
Ta1 O6 Pr2 147.1(2) . 2 ?
Pr1 O6 Pr2 110.06(18) 4_666 2 ?

_refine_diff_density_max         1.194
_refine_diff_density_min         -0.999
_refine_diff_density_rms         0.262


# start Validation Reply Form
_vrf_PLAT430_3                   
;
PROBLEM: Short Inter D...A Contact  O5       ..O5       .       2.79 Ang.  
RESPONSE: This is not a D-H---A contact, and the distance reported in
this alert is simply an O---O interatomic distance.  The O5 atom has 
a satisfied bond valence sum, and does not support a hydrogen atom in
this dense structure.
;
####################################################################### 
# 
# 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 1888863'
loop_
_audit_author_name
_audit_author_address
'Colin McMillen'
;Clemson University
United States of America
;
_audit_update_record             
;
2019-01-04 deposited with the CCDC.	2019-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'H O10 Pr3 Ta2'
_chemical_formula_weight         945.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_H-M_alt        'P n n m'
_space_group_name_Hall           '-P 2 2n'

_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, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   19.3603(10)
_cell_length_b                   5.5779(3)
_cell_length_c                   7.7079(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     832.37(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    5139
_cell_measurement_theta_min      2.84
_cell_measurement_theta_max      30.49

_exptl_crystal_description       column
_exptl_crystal_colour            green
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    .
_exptl_crystal_density_diffrn    7.546
_exptl_crystal_F_000             1616
_exptl_transmission_factor_min   .
_exptl_transmission_factor_max   .
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    43.454
_shelx_estimated_absorpt_T_min   0.098
_shelx_estimated_absorpt_T_max   0.180
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4857
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'SADABS, Bruker'
_exptl_absorpt_special_details   .
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   Ius
_diffrn_measurement_device_type  'Bruker Photon 100'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean .
_diffrn_reflns_number            14191
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.104
_diffrn_reflns_theta_max         25.490
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             840
_reflns_number_gt                754
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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 APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT-2014 (Sheldrick 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND (Bradenburg, 1999)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0213P)²+7.7583P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.00039(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         840
_refine_ls_number_parameters     79
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0208
_refine_ls_wR_factor_ref         0.0452
_refine_ls_wR_factor_gt          0.0434
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.000
_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_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
Pr1 Pr 0.14301(3) 0.42300(12) 0.000000 0.01845(18) Uani 1 2 d S T P . .
Pr2 Pr 0.09694(3) -0.50859(12) 0.500000 0.01827(18) Uani 1 2 d S T P . .
Pr3 Pr 0.000000 0.000000 0.25730(8) 0.01928(17) Uani 1 2 d S T P . .
Ta1 Ta 0.18283(2) -0.07895(6) 0.25181(4) 0.01668(13) Uani 1 1 d . . . . .
O1 O 0.2680(3) 0.1009(10) 0.3000(7) 0.0192(12) Uani 1 1 d . . . . .
O2 O -0.0020(4) -0.7461(15) 0.500000 0.0229(18) Uani 1 2 d S T P . .
O3 O 0.1794(4) -0.1738(15) 0.500000 0.0173(17) Uani 1 2 d S T P . .
O4 O 0.1227(3) 0.1912(10) 0.2796(7) 0.0205(13) Uani 1 1 d . . . . .
O5 O 0.0998(3) -0.2839(10) 0.2133(7) 0.0198(13) Uani 1 1 d . . . . .
O6 O 0.0269(4) 0.2555(14) 0.000000 0.0216(18) Uani 1 2 d DS T P . .
H6 H 0.045850 0.099463 0.000000 0.020 Uiso 1 2 d DS U P . .
O7 O 0.1889(4) 0.0045(15) 0.000000 0.0213(19) Uani 1 2 d S T 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
Pr1 O6 2.434(8) . ?
Pr1 O5 2.465(6) 1_565 ?
Pr1 O5 2.465(6) 6_565 ?
Pr1 O7 2.497(9) . ?
Pr1 O1 2.516(6) 3 ?
Pr1 O1 2.516(6) 8_665 ?
Pr1 O4 2.544(5) . ?
Pr1 O4 2.544(5) 6 ?
Pr1 Ta1 3.4755(6) 1_565 ?
Pr1 Ta1 3.4755(6) 6_565 ?
Pr1 Ta1 3.4930(7) 6 ?
Pr1 Ta1 3.4930(7) . ?
Pr2 O2 2.322(9) 5_546 ?
Pr2 O2 2.330(9) . ?
Pr2 O4 2.437(6) 1_545 ?
Pr2 O4 2.437(6) 6_546 ?
Pr2 O3 2.457(8) . ?
Pr2 O5 2.541(6) . ?
Pr2 O5 2.541(6) 6_556 ?
Pr2 Ta1 3.4882(6) 6_556 ?
Pr2 Ta1 3.4883(6) . ?
Pr2 Pr2 3.7548(13) 5_546 ?
Pr2 Pr3 3.8125(7) 1_545 ?
Pr2 Pr3 3.8125(7) 5_546 ?
Pr3 O2 2.347(5) 1_565 ?
Pr3 O2 2.347(5) 5_546 ?
Pr3 O6 2.497(5) . ?
Pr3 O6 2.497(5) 5 ?
Pr3 O5 2.521(6) . ?
Pr3 O5 2.521(6) 2 ?
Pr3 O4 2.609(6) 2 ?
Pr3 O4 2.610(6) . ?
Pr3 Ta1 3.5672(4) 2 ?
Pr3 Ta1 3.5673(4) . ?
Pr3 Pr3 3.7414(12) 5_556 ?
Ta1 O4 1.917(6) . ?
Ta1 O1 1.966(5) . ?
Ta1 O3 1.986(2) . ?
Ta1 O5 1.995(5) . ?
Ta1 O7 1.999(2) . ?
Ta1 O1 2.062(5) 3_545 ?

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
O6 Pr1 O5 86.61(19) . 1_565 ?
O6 Pr1 O5 86.61(19) . 6_565 ?
O5 Pr1 O5 83.7(3) 1_565 6_565 ?
O6 Pr1 O7 88.3(3) . . ?
O5 Pr1 O7 137.78(14) 1_565 . ?
O5 Pr1 O7 137.78(14) 6_565 . ?
O6 Pr1 O1 141.60(13) . 3 ?
O5 Pr1 O1 64.04(18) 1_565 3 ?
O5 Pr1 O1 112.31(19) 6_565 3 ?
O7 Pr1 O1 97.20(19) . 3 ?
O6 Pr1 O1 141.60(13) . 8_665 ?
O5 Pr1 O1 112.31(19) 1_565 8_665 ?
O5 Pr1 O1 64.04(18) 6_565 8_665 ?
O7 Pr1 O1 97.20(19) . 8_665 ?
O1 Pr1 O1 75.6(3) 3 8_665 ?
O6 Pr1 O4 70.25(15) . . ?
O5 Pr1 O4 73.70(19) 1_565 . ?
O5 Pr1 O4 148.17(19) 6_565 . ?
O7 Pr1 O4 65.16(15) . . ?
O1 Pr1 O4 77.72(18) 3 . ?
O1 Pr1 O4 145.64(19) 8_665 . ?
O6 Pr1 O4 70.25(15) . 6 ?
O5 Pr1 O4 148.17(19) 1_565 6 ?
O5 Pr1 O4 73.70(19) 6_565 6 ?
O7 Pr1 O4 65.16(15) . 6 ?
O1 Pr1 O4 145.65(19) 3 6 ?
O1 Pr1 O4 77.72(18) 8_665 6 ?
O4 Pr1 O4 115.8(3) . 6 ?
O6 Pr1 Ta1 120.77(14) . 1_565 ?
O5 Pr1 Ta1 34.19(13) 1_565 1_565 ?
O5 Pr1 Ta1 85.28(14) 6_565 1_565 ?
O7 Pr1 Ta1 131.93(13) . 1_565 ?
O1 Pr1 Ta1 35.96(12) 3 1_565 ?
O1 Pr1 Ta1 82.82(13) 8_665 1_565 ?
O4 Pr1 Ta1 88.13(13) . 1_565 ?
O4 Pr1 Ta1 156.02(13) 6 1_565 ?
O6 Pr1 Ta1 120.77(14) . 6_565 ?
O5 Pr1 Ta1 85.28(14) 1_565 6_565 ?
O5 Pr1 Ta1 34.19(13) 6_565 6_565 ?
O7 Pr1 Ta1 131.93(13) . 6_565 ?
O1 Pr1 Ta1 82.82(13) 3 6_565 ?
O1 Pr1 Ta1 35.96(12) 8_665 6_565 ?
O4 Pr1 Ta1 156.02(13) . 6_565 ?
O4 Pr1 Ta1 88.13(13) 6 6_565 ?
Ta1 Pr1 Ta1 67.899(16) 1_565 6_565 ?
O6 Pr1 Ta1 84.04(15) . 6 ?
O5 Pr1 Ta1 167.73(13) 1_565 6 ?
O5 Pr1 Ta1 103.64(14) 6_565 6 ?
O7 Pr1 Ta1 34.14(3) . 6 ?
O1 Pr1 Ta1 120.37(13) 3 6 ?
O1 Pr1 Ta1 79.90(13) 8_665 6 ?
O4 Pr1 Ta1 95.60(13) . 6 ?
O4 Pr1 Ta1 32.43(13) 6 6 ?
Ta1 Pr1 Ta1 154.43(2) 1_565 6 ?
Ta1 Pr1 Ta1 106.347(11) 6_565 6 ?
O6 Pr1 Ta1 84.04(15) . . ?
O5 Pr1 Ta1 103.64(14) 1_565 . ?
O5 Pr1 Ta1 167.73(13) 6_565 . ?
O7 Pr1 Ta1 34.14(3) . . ?
O1 Pr1 Ta1 79.90(13) 3 . ?
O1 Pr1 Ta1 120.37(13) 8_665 . ?
O4 Pr1 Ta1 32.43(13) . . ?
O4 Pr1 Ta1 95.60(13) 6 . ?
Ta1 Pr1 Ta1 106.346(11) 1_565 . ?
Ta1 Pr1 Ta1 154.43(2) 6_565 . ?
Ta1 Pr1 Ta1 67.513(16) 6 . ?
O2 Pr2 O2 72.4(3) 5_546 . ?
O2 Pr2 O4 125.60(17) 5_546 1_545 ?
O2 Pr2 O4 77.1(2) . 1_545 ?
O2 Pr2 O4 125.60(17) 5_546 6_546 ?
O2 Pr2 O4 77.1(2) . 6_546 ?
O4 Pr2 O4 88.4(2) 1_545 6_546 ?
O2 Pr2 O3 92.8(3) 5_546 . ?
O2 Pr2 O3 165.2(3) . . ?
O4 Pr2 O3 112.90(19) 1_545 . ?
O4 Pr2 O3 112.90(19) 6_546 . ?
O2 Pr2 O5 73.46(15) 5_546 . ?
O2 Pr2 O5 107.35(15) . . ?
O4 Pr2 O5 74.23(18) 1_545 . ?
O4 Pr2 O5 160.18(18) 6_546 . ?
O3 Pr2 O5 67.12(14) . . ?
O2 Pr2 O5 73.46(15) 5_546 6_556 ?
O2 Pr2 O5 107.35(15) . 6_556 ?
O4 Pr2 O5 160.18(18) 1_545 6_556 ?
O4 Pr2 O5 74.23(18) 6_546 6_556 ?
O3 Pr2 O5 67.12(14) . 6_556 ?
O5 Pr2 O5 120.8(2) . 6_556 ?
O2 Pr2 Ta1 87.53(18) 5_546 6_556 ?
O2 Pr2 Ta1 141.52(10) . 6_556 ?
O4 Pr2 Ta1 139.19(14) 1_545 6_556 ?
O4 Pr2 Ta1 89.55(13) 6_546 6_556 ?
O3 Pr2 Ta1 33.70(3) . 6_556 ?
O5 Pr2 Ta1 97.35(12) . 6_556 ?
O5 Pr2 Ta1 34.31(12) 6_556 6_556 ?
O2 Pr2 Ta1 87.53(18) 5_546 . ?
O2 Pr2 Ta1 141.52(10) . . ?
O4 Pr2 Ta1 89.55(13) 1_545 . ?
O4 Pr2 Ta1 139.19(14) 6_546 . ?
O3 Pr2 Ta1 33.70(3) . . ?
O5 Pr2 Ta1 34.31(12) . . ?
O5 Pr2 Ta1 97.35(12) 6_556 . ?
Ta1 Pr2 Ta1 66.518(16) 6_556 . ?
O2 Pr2 Pr2 36.2(2) 5_546 5_546 ?
O2 Pr2 Pr2 36.1(2) . 5_546 ?
O4 Pr2 Pr2 102.83(14) 1_545 5_546 ?
O4 Pr2 Pr2 102.83(14) 6_546 5_546 ?
O3 Pr2 Pr2 129.1(2) . 5_546 ?
O5 Pr2 Pr2 90.51(13) . 5_546 ?
O5 Pr2 Pr2 90.51(13) 6_556 5_546 ?
Ta1 Pr2 Pr2 117.32(2) 6_556 5_546 ?
Ta1 Pr2 Pr2 117.32(2) . 5_546 ?
O2 Pr2 Pr3 92.89(18) 5_546 1_545 ?
O2 Pr2 Pr3 35.53(12) . 1_545 ?
O4 Pr2 Pr3 42.66(14) 1_545 1_545 ?
O4 Pr2 Pr3 87.07(13) 6_546 1_545 ?
O3 Pr2 Pr3 150.04(4) . 1_545 ?
O5 Pr2 Pr3 86.47(12) . 1_545 ?
O5 Pr2 Pr3 142.36(12) 6_556 1_545 ?
Ta1 Pr2 Pr3 176.114(15) 6_556 1_545 ?
Ta1 Pr2 Pr3 117.355(10) . 1_545 ?
Pr2 Pr2 Pr3 61.721(16) 5_546 1_545 ?
O2 Pr2 Pr3 92.89(18) 5_546 5_546 ?
O2 Pr2 Pr3 35.53(11) . 5_546 ?
O4 Pr2 Pr3 87.07(13) 1_545 5_546 ?
O4 Pr2 Pr3 42.66(14) 6_546 5_546 ?
O3 Pr2 Pr3 150.04(4) . 5_546 ?
O5 Pr2 Pr3 142.36(12) . 5_546 ?
O5 Pr2 Pr3 86.47(12) 6_556 5_546 ?
Ta1 Pr2 Pr3 117.355(10) 6_556 5_546 ?
Ta1 Pr2 Pr3 176.114(15) . 5_546 ?
Pr2 Pr2 Pr3 61.721(16) 5_546 5_546 ?
Pr3 Pr2 Pr3 58.770(19) 1_545 5_546 ?
O2 Pr3 O2 74.3(3) 1_565 5_546 ?
O2 Pr3 O6 107.0(2) 1_565 . ?
O2 Pr3 O6 166.9(3) 5_546 . ?
O2 Pr3 O6 166.9(3) 1_565 5 ?
O2 Pr3 O6 107.0(2) 5_546 5 ?
O6 Pr3 O6 74.9(3) . 5 ?
O2 Pr3 O5 120.0(2) 1_565 . ?
O2 Pr3 O5 73.4(2) 5_546 . ?
O6 Pr3 O5 95.3(2) . . ?
O6 Pr3 O5 72.2(2) 5 . ?
O2 Pr3 O5 73.4(2) 1_565 2 ?
O2 Pr3 O5 120.0(2) 5_546 2 ?
O6 Pr3 O5 72.2(2) . 2 ?
O6 Pr3 O5 95.3(2) 5 2 ?
O5 Pr3 O5 164.5(3) . 2 ?
O2 Pr3 O4 100.3(2) 1_565 2 ?
O2 Pr3 O4 73.5(2) 5_546 2 ?
O6 Pr3 O4 118.4(2) . 2 ?
O6 Pr3 O4 68.2(2) 5 2 ?
O5 Pr3 O4 116.71(18) . 2 ?
O5 Pr3 O4 64.42(18) 2 2 ?
O2 Pr3 O4 73.5(2) 1_565 . ?
O2 Pr3 O4 100.3(2) 5_546 . ?
O6 Pr3 O4 68.2(2) . . ?
O6 Pr3 O4 118.4(2) 5 . ?
O5 Pr3 O4 64.42(18) . . ?
O5 Pr3 O4 116.71(18) 2 . ?
O4 Pr3 O4 172.5(2) 2 . ?
O2 Pr3 Ta1 85.3(2) 1_565 2 ?
O2 Pr3 Ta1 95.8(2) 5_546 2 ?
O6 Pr3 Ta1 97.31(18) . 2 ?
O6 Pr3 Ta1 81.60(18) 5 2 ?
O5 Pr3 Ta1 146.75(12) . 2 ?
O5 Pr3 Ta1 32.91(12) 2 2 ?
O4 Pr3 Ta1 31.57(12) 2 2 ?
O4 Pr3 Ta1 148.60(12) . 2 ?
O2 Pr3 Ta1 95.8(2) 1_565 . ?
O2 Pr3 Ta1 85.3(2) 5_546 . ?
O6 Pr3 Ta1 81.60(18) . . ?
O6 Pr3 Ta1 97.31(18) 5 . ?
O5 Pr3 Ta1 32.91(12) . . ?
O5 Pr3 Ta1 146.75(12) 2 . ?
O4 Pr3 Ta1 148.60(12) 2 . ?
O4 Pr3 Ta1 31.57(12) . . ?
Ta1 Pr3 Ta1 178.64(2) 2 . ?
O2 Pr3 Pr3 37.14(17) 1_565 5_556 ?
O2 Pr3 Pr3 37.14(17) 5_546 5_556 ?
O6 Pr3 Pr3 142.57(15) . 5_556 ?
O6 Pr3 Pr3 142.57(14) 5 5_556 ?
O5 Pr3 Pr3 97.73(13) . 5_556 ?
O5 Pr3 Pr3 97.73(13) 2 5_556 ?
O4 Pr3 Pr3 86.23(12) 2 5_556 ?
O4 Pr3 Pr3 86.23(12) . 5_556 ?
Ta1 Pr3 Pr3 90.680(11) 2 5_556 ?
Ta1 Pr3 Pr3 90.680(11) . 5_556 ?
O2 Pr3 Pr2 35.2(2) 1_565 1_565 ?
O2 Pr3 Pr2 91.97(18) 5_546 1_565 ?
O6 Pr3 Pr2 82.91(15) . 1_565 ?
O6 Pr3 Pr2 154.53(16) 5 1_565 ?
O5 Pr3 Pr2 98.08(12) . 1_565 ?
O5 Pr3 Pr2 89.51(13) 2 1_565 ?
O4 Pr3 Pr2 135.21(12) 2 1_565 ?
O4 Pr3 Pr2 39.26(12) . 1_565 ?
Ta1 Pr3 Pr2 113.924(13) 2 1_565 ?
Ta1 Pr3 Pr2 66.804(12) . 1_565 ?
Pr3 Pr3 Pr2 60.615(10) 5_556 1_565 ?
O4 Ta1 O1 95.0(2) . . ?
O4 Ta1 O3 94.7(3) . . ?
O1 Ta1 O3 89.0(3) . . ?
O4 Ta1 O5 88.7(2) . . ?
O1 Ta1 O5 175.3(2) . . ?
O3 Ta1 O5 87.9(3) . . ?
O4 Ta1 O7 87.8(3) . . ?
O1 Ta1 O7 90.9(3) . . ?
O3 Ta1 O7 177.6(3) . . ?
O5 Ta1 O7 92.1(3) . . ?
O4 Ta1 O1 169.4(2) . 3_545 ?
O1 Ta1 O1 95.25(10) . 3_545 ?
O3 Ta1 O1 88.4(3) . 3_545 ?
O5 Ta1 O1 81.2(2) . 3_545 ?
O7 Ta1 O1 89.2(3) . 3_545 ?
O4 Ta1 Pr1 123.79(17) . 1_545 ?
O1 Ta1 Pr1 134.40(17) . 1_545 ?
O3 Ta1 Pr1 108.5(2) . 1_545 ?
O5 Ta1 Pr1 43.96(16) . 1_545 ?
O7 Ta1 Pr1 69.9(2) . 1_545 ?
O1 Ta1 Pr1 45.75(15) 3_545 1_545 ?
O4 Ta1 Pr2 100.92(17) . . ?
O1 Ta1 Pr2 130.31(16) . . ?
O3 Ta1 Pr2 43.4(2) . . ?
O5 Ta1 Pr2 45.87(17) . . ?
O7 Ta1 Pr2 136.1(2) . . ?
O1 Ta1 Pr2 74.42(16) 3_545 . ?
Pr1 Ta1 Pr2 69.598(12) 1_545 . ?
O4 Ta1 Pr1 45.38(16) . . ?
O1 Ta1 Pr1 83.17(16) . . ?
O3 Ta1 Pr1 137.9(2) . . ?
O5 Ta1 Pr1 101.46(17) . . ?
O7 Ta1 Pr1 44.5(2) . . ?
O1 Ta1 Pr1 133.49(16) 3_545 . ?
Pr1 Ta1 Pr1 106.346(11) 1_545 . ?
Pr2 Ta1 Pr1 138.608(18) . . ?
O4 Ta1 Pr3 45.47(18) . . ?
O1 Ta1 Pr3 140.10(17) . . ?
O3 Ta1 Pr3 89.3(2) . . ?
O5 Ta1 Pr3 43.34(16) . . ?
O7 Ta1 Pr3 92.3(2) . . ?
O1 Ta1 Pr3 124.55(16) 3_545 . ?
Pr1 Ta1 Pr3 83.408(15) 1_545 . ?
Pr2 Ta1 Pr3 66.751(14) . . ?
Pr1 Ta1 Pr3 71.857(14) . . ?
Ta1 O1 Ta1 142.4(3) . 3 ?
Ta1 O1 Pr1 119.3(2) . 3_545 ?
Ta1 O1 Pr1 98.3(2) 3 3_545 ?
Pr2 O2 Pr2 107.6(3) 5_546 . ?
Pr2 O2 Pr3 112.5(2) 5_546 1_545 ?
Pr2 O2 Pr3 109.2(3) . 1_545 ?
Pr2 O2 Pr3 112.5(2) 5_546 5_546 ?
Pr2 O2 Pr3 109.2(3) . 5_546 ?
Pr3 O2 Pr3 105.7(3) 1_545 5_546 ?
Ta1 O3 Ta1 148.8(4) . 6_556 ?
Ta1 O3 Pr2 102.9(2) . . ?
Ta1 O3 Pr2 102.9(2) 6_556 . ?
Ta1 O4 Pr2 137.9(3) . 1_565 ?
Ta1 O4 Pr1 102.2(2) . . ?
Pr2 O4 Pr1 105.9(2) 1_565 . ?
Ta1 O4 Pr3 103.0(2) . . ?
Pr2 O4 Pr3 98.1(2) 1_565 . ?
Pr1 O4 Pr3 107.03(19) . . ?
Ta1 O5 Pr1 101.8(2) . 1_545 ?
Ta1 O5 Pr3 103.7(2) . . ?
Pr1 O5 Pr3 140.1(2) 1_545 . ?
Ta1 O5 Pr2 99.8(2) . . ?
Pr1 O5 Pr2 105.1(2) 1_545 . ?
Pr3 O5 Pr2 100.2(2) . . ?
Pr1 O6 Pr3 114.3(2) . . ?
Pr1 O6 Pr3 114.3(2) . 5 ?
Pr3 O6 Pr3 105.1(3) . 5 ?
Ta1 O7 Ta1 152.2(5) 6 . ?
Ta1 O7 Pr1 101.4(2) 6 . ?
Ta1 O7 Pr1 101.4(2) . . ?

_refine_diff_density_max         1.098
_refine_diff_density_min         -1.388
_refine_diff_density_rms         0.295


# start Validation Reply Form
_vrf_PLAT430_4                   
;
PROBLEM: Short Inter D...A Contact  O2       ..O2       .       2.83 Ang.  
RESPONSE: This is not a D-H---A contact, and the distance reported in
this alert is simply an O---O interatomic distance.  The O2 atom has 
a satisfied bond valence sum, and does not support a hydrogen atom in
this dense structure.
;
