#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/52/4335222.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4335222
loop_
_publ_author_name
'Karah E. Knope'
'L. Soderholm'
_publ_contact_author_address
;
Chemical Sciences and Engineering Division
Argonne National Laboratory
9700 South Cass Avenue
Argonne, IL 60439
;
_publ_contact_author_email       kknope@anl.gov
_publ_contact_author_name        'K.E. Knope'
_publ_contact_author_phone       630-252-0957
_publ_section_title
;
 Plutonium(IV) Cluster with a Hexanuclear [Pu6(OH)4O4]12+ Core
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6770
_journal_page_last               6772
_journal_paper_doi               10.1021/ic4007185
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety
' Li6Pu6(OH)4O4(H2O)6(H3NCH2CO2)12,10.5(H2O),Cl18'
_chemical_formula_sum            'C24 H97 Cl18 Li6 N12 O48.5 Pu6'
_chemical_formula_weight         3461.88
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   22.497(2)
_cell_length_b                   22.497(2)
_cell_length_c                   15.1236(15)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.49
_cell_volume                     6628.8(11)
_computing_cell_refinement       'Bruker Apex2'
_computing_data_collection       'Bruker Apex2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    CrystalMaker
_computing_publication_material  'WinGX v1.80.05'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'bruker Apex II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25140
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    5.049
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.602
_exptl_crystal_description       plate
_exptl_crystal_F_000             4803
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.306
_refine_diff_density_min         -0.957
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         3038
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0220
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0150P)²+79.8309P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0434
_refine_ls_wR_factor_ref         0.0454
_reflns_number_gt                2646
_reflns_number_total             3038
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4007185_si_002.cif
_cod_data_source_block           compound
_cod_original_cell_volume        6628.6(11)
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'C24 H97 Cl18 Li6 N12 O48.50 Pu6'
_cod_database_code               4335222
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pu1 Pu 0.967572(8) 0.891264(8) 0.101858(10) 0.00955(5) Uani 1 1 d .
O1 O 0.9700(2) 0.8951(3) -0.0501(3) 0.0600(16) Uani 1 1 d U
O2 O 1.0000 1.0000 0.1496(6) 0.050(2) Uani 1 3 d SU
O3 O 0.92846(18) 0.77775(17) 0.1994(2) 0.0156(7) Uani 1 1 d .
O4 O 1.02232(17) 0.82548(16) 0.0721(2) 0.0165(7) Uani 1 1 d .
O5 O 0.87198(18) 0.78865(17) 0.0516(2) 0.0260(8) Uani 1 1 d .
C10 C 1.0627(3) 0.8298(3) 0.0117(3) 0.0187(10) Uani 1 1 d .
C11 C 1.0909(3) 0.7818(3) 0.0138(4) 0.0269(12) Uani 1 1 d .
H11A H 1.0811 0.7574 -0.0421 0.032 Uiso 1 1 calc R
H11B H 1.1403 0.8081 0.0208 0.032 Uiso 1 1 calc R
N12 N 1.0611(2) 0.7316(2) 0.0867(3) 0.0200(9) Uani 1 1 d .
O6 O 0.89318(17) 0.87409(17) 0.2277(2) 0.0178(7) Uani 1 1 d .
O7 O 1.04351(16) 0.90807(16) 0.2304(2) 0.0149(7) Uani 1 1 d .
C20 C 0.8621(2) 0.9026(2) 0.2590(3) 0.0155(10) Uani 1 1 d .
C21 C 0.8175(3) 0.8716(2) 0.3404(3) 0.0194(10) Uani 1 1 d .
H21A H 0.8337 0.9056 0.3873 0.023 Uiso 1 1 calc R
H21B H 0.7707 0.8594 0.3265 0.023 Uiso 1 1 calc R
N22 N 0.8186(2) 0.8095(2) 0.3719(3) 0.0195(9) Uani 1 1 d .
Cl1 Cl 0.95908(6) 0.81655(6) 0.42564(8) 0.0211(3) Uani 1 1 d .
Cl2 Cl 1.06830(6) 0.76409(6) 0.29085(8) 0.0218(3) Uani 1 1 d .
Cl3 Cl 0.76653(6) 0.69251(6) 0.23103(9) 0.0255(3) Uani 1 1 d .
Li1 Li 1.0016(4) 0.8163(4) 0.2850(5) 0.0204(18) Uani 1 1 d .
OW1 O 0.9503(4) 0.7600(4) -0.1196(5) 0.0312(18) Uani 0.50 1 d P
OW2 O 0.8595(5) 0.6286(5) -0.1698(6) 0.037(2) Uani 0.50 1 d P
OW3 O 0.9037(6) 0.6498(6) -0.1580(6) 0.047(3) Uani 0.50 1 d P
OW4 O 0.988(3) 0.9740(11) 0.3618(17) 0.086(11) Uani 0.25 1 d P
H3A H 0.890(3) 0.764(3) 0.213(4) 0.028(17) Uiso 1 1 d .
H3B H 0.929(4) 0.747(4) 0.165(5) 0.07(3) Uiso 1 1 d .
H12A H 1.081(3) 0.701(3) 0.087(4) 0.048(19) Uiso 1 1 d .
H12B H 1.011(4) 0.700(4) 0.084(5) 0.06(2) Uiso 1 1 d .
H12C H 1.073(4) 0.755(4) 0.145(5) 0.07(2) Uiso 1 1 d .
H22A H 0.863(3) 0.824(3) 0.384(3) 0.015(13) Uiso 1 1 d .
H22B H 0.800(4) 0.773(4) 0.330(5) 0.07(2) Uiso 1 1 d .
H22C H 0.796(4) 0.799(3) 0.423(5) 0.05(2) Uiso 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O1 Pu1 O2 69.33(17) 11_565 .
O1 Pu1 O1 69.40(17) 11_565 .
O2 Pu1 O1 106.6(3) . .
O1 Pu1 O1 106.2(3) 11_565 12_655
O2 Pu1 O1 68.55(16) . 12_655
O1 Pu1 O1 68.62(17) . 12_655
O1 Pu1 O5 76.10(16) 11_565 .
O2 Pu1 O5 142.54(10) . .
O1 Pu1 O5 73.00(15) . .
O1 Pu1 O5 137.33(13) 12_655 .
O1 Pu1 O4 145.61(12) 11_565 .
O2 Pu1 O4 137.00(8) . .
O1 Pu1 O4 79.95(15) . .
O1 Pu1 O4 75.29(15) 12_655 .
O5 Pu1 O4 80.42(12) . .
O1 Pu1 O6 76.66(15) 11_565 .
O2 Pu1 O6 75.5(2) . .
O1 Pu1 O6 142.07(12) . .
O1 Pu1 O6 139.55(12) 12_655 .
O5 Pu1 O6 83.03(12) . .
O4 Pu1 O6 125.05(10) . .
O1 Pu1 O7 140.93(12) 11_565 .
O2 Pu1 O7 76.33(19) . .
O1 Pu1 O7 140.66(12) . .
O1 Pu1 O7 76.85(15) 12_655 .
O5 Pu1 O7 128.39(11) . .
O4 Pu1 O7 73.42(11) . .
O6 Pu1 O7 77.22(11) . .
O1 Pu1 O3 124.23(17) 11_565 .
O2 Pu1 O3 128.3(2) . .
O1 Pu1 O3 125.08(17) . .
O1 Pu1 O3 129.54(17) 12_655 .
O5 Pu1 O3 62.75(11) . .
O4 Pu1 O3 62.69(11) . .
O6 Pu1 O3 63.11(11) . .
O7 Pu1 O3 65.76(10) . .
O1 Pu1 Li1 143.3(2) 11_565 .
O2 Pu1 Li1 103.5(3) . .
O1 Pu1 Li1 142.92(19) . .
O1 Pu1 Li1 103.9(2) 12_655 .
O5 Pu1 Li1 95.45(15) . .
O4 Pu1 Li1 63.23(15) . .
O6 Pu1 Li1 66.78(16) . .
O7 Pu1 Li1 32.98(15) . .
O3 Pu1 Li1 32.79(15) . .
O1 Pu1 Pu1 34.65(11) 11_565 3_675
O2 Pu1 Pu1 34.72(11) . 3_675
O1 Pu1 Pu1 88.81(14) . 3_675
O1 Pu1 Pu1 88.13(14) 12_655 3_675
O5 Pu1 Pu1 109.26(9) . 3_675
O4 Pu1 Pu1 162.46(8) . 3_675
O6 Pu1 Pu1 71.62(7) . 3_675
O7 Pu1 Pu1 108.74(7) . 3_675
O3 Pu1 Pu1 134.55(8) . 3_675
Li1 Pu1 Pu1 127.97(13) . 3_675
O1 Pu1 Pu1 88.79(14) 11_565 2_765
O2 Pu1 Pu1 34.72(11) . 2_765
O1 Pu1 Pu1 88.13(14) . 2_765
O1 Pu1 Pu1 33.87(11) 12_655 2_765
O5 Pu1 Pu1 158.97(8) . 2_765
O4 Pu1 Pu1 105.84(8) . 2_765
O6 Pu1 Pu1 107.95(8) . 2_765
O7 Pu1 Pu1 72.35(7) . 2_765
O3 Pu1 Pu1 138.11(7) . 2_765
Li1 Pu1 Pu1 105.33(13) . 2_765
Pu1 Pu1 Pu1 60.0 3_675 2_765
Pu1 O1 Pu1 111.73(19) 12_655 .
Pu1 O1 Pu1 111.49(19) 12_655 11_565
Pu1 O1 Pu1 110.08(19) . 11_565
Pu1 O2 Pu1 110.6(2) 3_675 .
Pu1 O2 Pu1 110.5(2) 3_675 2_765
Pu1 O2 Pu1 110.6(2) . 2_765
Li1 O3 Pu1 98.1(3) . .
Li1 O3 H3A 122(4) . .
Pu1 O3 H3A 107(4) . .
Li1 O3 H3B 114(5) . .
Pu1 O3 H3B 108(5) . .
H3A O3 H3B 107(6) . .
C10 O4 Pu1 131.6(3) . .
C10 O5 Pu1 139.7(3) 11_565 .
O4 C10 O5 126.1(4) . 12_655
O4 C10 C11 118.5(4) . .
O5 C10 C11 115.3(4) 12_655 .
N12 C11 C10 111.8(4) . .
N12 C11 H11A 109.3 . .
C10 C11 H11A 109.3 . .
N12 C11 H11B 109.3 . .
C10 C11 H11B 109.3 . .
H11A C11 H11B 107.9 . .
C11 N12 H12A 110(4) . .
C11 N12 H12B 116(4) . .
H12A N12 H12B 104(6) . .
C11 N12 H12C 111(4) . .
H12A N12 H12C 106(6) . .
H12B N12 H12C 109(6) . .
C20 O6 Pu1 136.8(3) . .
C20 O7 Li1 123.6(4) 2_765 .
C20 O7 Pu1 132.8(3) 2_765 .
Li1 O7 Pu1 103.6(3) . .
O6 C20 O7 126.4(4) . 3_675
O6 C20 C21 118.6(4) . .
O7 C20 C21 114.9(4) 3_675 .
N22 C21 C20 112.0(4) . .
N22 C21 H21A 109.2 . .
C20 C21 H21A 109.2 . .
N22 C21 H21B 109.2 . .
C20 C21 H21B 109.2 . .
H21A C21 H21B 107.9 . .
C21 N22 H22A 105(3) . .
C21 N22 H22B 113(5) . .
H22A N22 H22B 112(5) . .
C21 N22 H22C 105(4) . .
H22A N22 H22C 108(5) . .
H22B N22 H22C 113(6) . .
O3 Li1 O7 92.5(4) . .
O3 Li1 Cl2 114.9(4) . .
O7 Li1 Cl2 117.0(4) . .
O3 Li1 Cl1 110.8(4) . .
O7 Li1 Cl1 111.2(4) . .
Cl2 Li1 Cl1 109.6(3) . .
O3 Li1 Pu1 49.1(2) . .
O7 Li1 Pu1 43.38(19) . .
Cl2 Li1 Pu1 128.5(3) . .
Cl1 Li1 Pu1 121.9(3) . .
OW4 OW4 OW4 59.99(5) 3_675 2_765
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pu1 O1 2.256(4) 11_565
Pu1 O2 2.292(3) .
Pu1 O1 2.300(4) .
Pu1 O1 2.302(4) 12_655
Pu1 O5 2.360(3) .
Pu1 O4 2.394(3) .
Pu1 O6 2.434(3) .
Pu1 O7 2.489(3) .
Pu1 O3 2.688(3) .
Pu1 Li1 3.521(8) .
Pu1 Pu1 3.7675(5) 3_675
Pu1 Pu1 3.7676(5) 2_765
O1 Pu1 2.256(4) 12_655
O1 Pu1 2.302(4) 11_565
O2 Pu1 2.292(3) 3_675
O2 Pu1 2.292(3) 2_765
O3 Li1 1.926(9) .
O3 H3A 0.79(6) .
O3 H3B 0.87(8) .
O4 C10 1.257(5) .
O5 C10 1.261(6) 11_565
C10 O5 1.261(6) 12_655
C10 C11 1.503(7) .
C11 N12 1.477(6) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
N12 H12A 0.98(7) .
N12 H12B 0.98(8) .
N12 H12C 1.00(8) .
O6 C20 1.255(5) .
O7 C20 1.261(6) 2_765
O7 Li1 1.972(9) .
C20 O7 1.261(5) 3_675
C20 C21 1.519(6) .
C21 N22 1.487(6) .
C21 H21A 0.9700 .
C21 H21B 0.9700 .
N22 H22A 0.91(5) .
N22 H22B 0.95(8) .
N22 H22C 0.89(7) .
Cl1 Li1 2.333(8) .
Cl2 Li1 2.323(9) .
OW2 OW3 0.880(11) .
OW4 OW4 0.88(4) 3_675
OW4 OW4 0.88(4) 2_765
