# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_April2023_P3_b
_database_code_depnum_ccdc_archive 'CCDC 2190098'
loop_
_audit_author_name
_audit_author_address
'Ginger E. Sigmon'
;University of Notre Dame
United States of America
;
_audit_update_record             
;
2023-06-07 deposited with the CCDC.	2023-08-08 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT213_April2023_P3_b      
;
PROBLEM: Atom O1              has ADP max/min Ratio .....        5.1 prolat
RESPONSE: Displacement ellipsoid of O001 site is elongated along three-fold axes due to disorder. 
;
_vrf_PLAT306_April2023_P3_b      
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O6 Check 
RESPONSE: O006 site is an oxygen atom of a water molecule. 
;
# end Validation Reply Form



_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B2 O17 P3 Pu'
_chemical_formula_weight         628.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 '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'
Pu Pu -9.4100 4.3056 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           143
_space_group_name_H-M_alt        'P 3'
_space_group_name_Hall           'P 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'
'-y, x-y, z'
'-x+y, -x, z'

_cell_length_a                   7.8764(10)
_cell_length_b                   7.8764(10)
_cell_length_c                   5.5355(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     297.40(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    3813
_cell_measurement_theta_min      2.99
_cell_measurement_theta_max      29.13

_exptl_crystal_description       blocky
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    3.509
_exptl_crystal_F_000             285
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.025
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    6.051
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.624
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  Bruker
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3813
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         2.986
_diffrn_reflns_theta_max         29.148
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1015
_reflns_number_gt                1015
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.930
_reflns_Friedel_fraction_max     0.891
_reflns_Friedel_fraction_full    0.997

_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    CrystalMaker
_computing_publication_material  ?
_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)+(0.0260P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   none
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 488 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.028(14)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1015
_refine_ls_number_parameters     70
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0181
_refine_ls_R_factor_gt           0.0181
_refine_ls_wR_factor_ref         0.0446
_refine_ls_wR_factor_gt          0.0446
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.084
_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
Pu01 Pu 1.000000 1.000000 0.20881(2) 0.00672(12) Uani 1 3 d S T P . .
P001 P 0.6954(3) 1.0047(3) 0.7083(3) 0.0081(4) Uani 1 1 d . . . . .
O1 O 0.2615(10) 0.4697(9) 0.698(2) 0.046(2) Uani 1 1 d . . . . .
O2 O 0.8683(8) 0.4615(8) 0.7094(11) 0.0132(11) Uani 1 1 d . . . . .
O3 O 0.333333 0.666667 0.366(2) 0.029(3) Uani 1 3 d S T P . .
O4 O 0.666667 0.333333 0.377(3) 0.035(3) Uani 1 3 d S T P . .
O5 O 0.8092(12) 1.0392(11) 0.9359(13) 0.0321(17) Uani 1 1 d . . . . .
O6 O 0.0275(12) 0.3602(10) 0.2175(14) 0.0306(17) Uani 1 1 d . . . . .
O7 O 0.8117(13) 1.0447(11) 0.4806(13) 0.0334(17) Uani 1 1 d . . . . .
B1 B 0.333333 0.666667 0.637(4) 0.015(3) Uani 1 3 d S T P . .
B2 B 0.666667 0.333333 0.646(5) 0.020(4) Uani 1 3 d S T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pu01 0.00784(14) 0.00784(14) 0.00446(17) 0.000 0.000 0.00392(7)
P001 0.0059(8) 0.0077(8) 0.0107(9) 0.0001(7) 0.0003(7) 0.0034(7)
O1 0.011(3) 0.006(3) 0.122(8) 0.003(4) -0.002(4) 0.005(3)
O2 0.010(2) 0.007(3) 0.021(3) -0.003(2) -0.002(2) 0.003(2)
O3 0.023(4) 0.023(4) 0.040(7) 0.000 0.000 0.0116(18)
O4 0.030(4) 0.030(4) 0.045(8) 0.000 0.000 0.015(2)
O5 0.046(5) 0.034(4) 0.029(4) -0.012(3) -0.026(3) 0.029(4)
O6 0.030(4) 0.018(3) 0.034(4) -0.005(3) -0.009(3) 0.004(3)
O7 0.044(5) 0.040(4) 0.026(4) 0.008(3) 0.020(3) 0.028(4)
B1 0.013(6) 0.013(6) 0.020(9) 0.000 0.000 0.006(3)
B2 0.013(6) 0.013(6) 0.035(12) 0.000 0.000 0.006(3)

_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
Pu01 O5 2.258(6) 2_764 ?
Pu01 O5 2.258(6) 1_554 ?
Pu01 O5 2.258(6) 3_674 ?
Pu01 O7 2.260(7) . ?
Pu01 O7 2.260(7) 3_675 ?
Pu01 O7 2.260(7) 2_765 ?
Pu01 O6 2.735(7) 2_665 ?
Pu01 O6 2.735(7) 1_665 ?
Pu01 O6 2.735(7) 3_665 ?
P001 O5 1.491(7) . ?
P001 O7 1.496(7) . ?
P001 O1 1.525(7) 2_665 ?
P001 O2 1.567(6) 3_675 ?
O1 B1 1.402(9) . ?
O2 B2 1.435(9) . ?
O3 B1 1.50(3) . ?
O4 B2 1.49(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Pu01 O5 80.1(3) 2_764 1_554 ?
O5 Pu01 O5 80.1(3) 2_764 3_674 ?
O5 Pu01 O5 80.1(3) 1_554 3_674 ?
O5 Pu01 O7 137.1(3) 2_764 . ?
O5 Pu01 O7 83.7(3) 1_554 . ?
O5 Pu01 O7 135.4(3) 3_674 . ?
O5 Pu01 O7 135.4(3) 2_764 3_675 ?
O5 Pu01 O7 137.1(3) 1_554 3_675 ?
O5 Pu01 O7 83.7(3) 3_674 3_675 ?
O7 Pu01 O7 80.5(3) . 3_675 ?
O5 Pu01 O7 83.7(3) 2_764 2_765 ?
O5 Pu01 O7 135.4(3) 1_554 2_765 ?
O5 Pu01 O7 137.1(3) 3_674 2_765 ?
O7 Pu01 O7 80.5(3) . 2_765 ?
O7 Pu01 O7 80.5(3) 3_675 2_765 ?
O5 Pu01 O6 65.4(2) 2_764 2_665 ?
O5 Pu01 O6 72.6(3) 1_554 2_665 ?
O5 Pu01 O6 138.7(3) 3_674 2_665 ?
O7 Pu01 O6 72.0(3) . 2_665 ?
O7 Pu01 O6 136.9(3) 3_675 2_665 ?
O7 Pu01 O6 62.9(3) 2_765 2_665 ?
O5 Pu01 O6 138.7(3) 2_764 1_665 ?
O5 Pu01 O6 65.4(2) 1_554 1_665 ?
O5 Pu01 O6 72.6(3) 3_674 1_665 ?
O7 Pu01 O6 62.9(3) . 1_665 ?
O7 Pu01 O6 72.0(3) 3_675 1_665 ?
O7 Pu01 O6 136.9(3) 2_765 1_665 ?
O6 Pu01 O6 119.969(12) 2_665 1_665 ?
O5 Pu01 O6 72.6(3) 2_764 3_665 ?
O5 Pu01 O6 138.7(3) 1_554 3_665 ?
O5 Pu01 O6 65.4(2) 3_674 3_665 ?
O7 Pu01 O6 136.9(3) . 3_665 ?
O7 Pu01 O6 62.9(3) 3_675 3_665 ?
O7 Pu01 O6 72.0(3) 2_765 3_665 ?
O6 Pu01 O6 119.969(11) 2_665 3_665 ?
O6 Pu01 O6 119.969(13) 1_665 3_665 ?
O5 P001 O7 115.1(5) . . ?
O5 P001 O1 109.6(5) . 2_665 ?
O7 P001 O1 107.3(5) . 2_665 ?
O5 P001 O2 109.5(4) . 3_675 ?
O7 P001 O2 109.0(4) . 3_675 ?
O1 P001 O2 105.9(3) 2_665 3_675 ?
B1 O1 P001 144.9(6) . 3_565 ?
B2 O2 P001 130.8(5) . 2_765 ?
P001 O5 Pu01 157.1(4) . 1_556 ?
P001 O7 Pu01 155.3(5) . . ?
O1 B1 O1 114.4(8) 3_565 2_665 ?
O1 B1 O1 114.4(8) 3_565 . ?
O1 B1 O1 114.4(8) 2_665 . ?
O1 B1 O3 104.0(10) 3_565 . ?
O1 B1 O3 104.0(10) 2_665 . ?
O1 B1 O3 104.0(10) . . ?
O2 B2 O2 114.3(8) 3_665 2_655 ?
O2 B2 O2 114.3(8) 3_665 . ?
O2 B2 O2 114.3(8) 2_655 . ?
O2 B2 O4 104.1(11) 3_665 . ?
O2 B2 O4 104.1(11) 2_655 . ?
O2 B2 O4 104.1(11) . . ?

_refine_diff_density_max         1.351
_refine_diff_density_min         -1.363
_refine_diff_density_rms         0.192

_shelx_res_file                  
;
TITL April2023_P3_b.res in P3
    April2023_P3_b.res
    created by SHELXL-2018/3 at 16:59:08 on 19-Apr-2023
REM Old TITL April2023_P3 in P3

REM SHELXT solution in P3
REM R1 0.044,  Rweak 0.326,  Alpha 0.016,  Orientation as input
REM Flack x =  0.496 ( 0.037 ) from Parsons' quotients
REM Formula found by SHELXT:  B15 O11 P3 Pu

CELL  0.71073   7.8764   7.8764   5.5355   90.000   90.000  120.000
ZERR    1.000   0.0010   0.0010   0.0007    0.000    0.000    0.000
LATT -1
SYMM -Y, X-Y, Z
SYMM -X+Y, -X, Z
SFAC B O P PU
UNIT 2 17 3 1
TEMP 0.000
L.S. 10
BOND
LIST 4
FMAP 2
PLAN 20
ACTA
WGHT    0.026000
FVAR       0.85457
PU01  4    1.000000    1.000000    0.208813    10.33333    0.00784    0.00784 =
         0.00446    0.00000    0.00000    0.00392
P001  3    0.695375    1.004691    0.708272    11.00000    0.00587    0.00767 =
         0.01072    0.00013    0.00025    0.00344
O1    2    0.261522    0.469672    0.698203    11.00000    0.01065    0.00618 =
         0.12207    0.00303   -0.00241    0.00464
O2    2    0.868280    0.461475    0.709385    11.00000    0.00955    0.00727 =
         0.02137   -0.00350   -0.00206    0.00312
O3    2    0.333333    0.666667    0.366382    10.33333    0.02318    0.02318 =
         0.04034    0.00000    0.00000    0.01159
O4    2    0.666667    0.333333    0.377161    10.33333    0.02967    0.02967 =
         0.04542    0.00000    0.00000    0.01484
O5    2    0.809238    1.039211    0.935865    11.00000    0.04551    0.03440 =
         0.02864   -0.01156   -0.02563    0.02913
O6    2    0.027511    0.360160    0.217545    11.00000    0.02987    0.01800 =
         0.03405   -0.00544   -0.00921    0.00450
O7    2    0.811746    1.044739    0.480648    11.00000    0.04402    0.03978 =
         0.02566    0.00754    0.02022    0.02788
B1    1    0.333333    0.666667    0.637025    10.33333    0.01265    0.01265 =
         0.01962    0.00000    0.00000    0.00632
B2    1    0.666667    0.333333    0.646139    10.33333    0.01252    0.01252 =
         0.03481    0.00000    0.00000    0.00626
HKLF 4




REM  April2023_P3_b.res in P3
REM wR2 = 0.044556, GooF = S = 1.08477, Restrained GooF = 1.08419 for all data
REM R1 = 0.018104 for 1015 Fo > 4sig(Fo) and 0.018104 for all 1015 data
REM 70 parameters refined using 1 restraints

END

WGHT      0.0261      0.0000

REM Highest difference peak  1.351,  deepest hole -1.363,  1-sigma level  0.192
Q1    1   0.3333  0.6667  0.0165  10.33333  0.05    1.35
Q2    1   0.6667  0.3333  0.0329  10.33333  0.05    1.18
Q3    1  -0.0017  0.3393  0.5431  11.00000  0.05    1.12
Q4    1   0.6565  1.0020  0.8798  11.00000  0.05    1.09
Q5    1   0.8089  0.2792  0.6087  11.00000  0.05    0.72
Q6    1   0.7369  0.5033  0.7825  11.00000  0.05    0.71
Q7    1   0.2857  0.4733  0.8095  11.00000  0.05    0.64
Q8    1   0.7930  0.8580  0.3655  11.00000  0.05    0.58
Q9    1   1.0000  1.0000  0.8429  10.33333  0.05    0.55
Q10   1  -0.0795  0.3226  0.3173  11.00000  0.05    0.51
Q11   1   0.2616  0.4702  0.1678  11.00000  0.05    0.48
Q12   1   0.8699  1.0562  1.0395  11.00000  0.05    0.47
Q13   1   0.7143  0.8631  0.4067  11.00000  0.05    0.47
Q14   1   0.5853  0.9114  1.1051  11.00000  0.05    0.47
Q15   1   0.1055  0.4183  0.3505  11.00000  0.05    0.47
Q16   1   0.1476  0.4773  0.2170  11.00000  0.05    0.45
Q17   1   0.8830  1.0638  0.8792  11.00000  0.05    0.44
Q18   1   0.4786  0.2143  0.2536  11.00000  0.05    0.44
Q19   1   0.7521  0.4641  0.1164  11.00000  0.05    0.44
Q20   1   0.7850  0.9317  0.6434  11.00000  0.05    0.43
;
_shelx_res_checksum              7522
