#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:10:58 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179097 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/59/4305984.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_4305984
loop_
_publ_author_name
'Andrew J. Gaunt'
'Sean D. Reilly'
'Alejandro E. Enriquez'
'Trevor W. Hayton'
'James M. Boncella'
'Brian L. Scott'
'Mary P. Neu'
_publ_section_title
;
Low-Valent Molecular Plutonium Halide Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8412
_journal_page_last               8419
_journal_paper_doi               10.1021/ic8009139
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C24 H48 Cl7 O6 Pu2'
_chemical_formula_weight         1164.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.186(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.1865(17)
_cell_length_b                   11.1628(15)
_cell_length_c                   13.9197(19)
_cell_measurement_temperature    141(2)
_cell_volume                     1835.8(4)
_computing_cell_refinement       'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_data_collection       'APEX II, v. 1.08 (Bruker AXS, 2003)'
_computing_data_reduction        'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_molecular_graphics    'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      141(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       'ω 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  0.0650
_diffrn_reflns_av_sigmaI/netI    0.0600
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21284
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.75
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.101
_exptl_absorpt_correction_T_max  0.9225
_exptl_absorpt_correction_T_min  0.6845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    2.107
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular slab'
_exptl_crystal_F_000             1094
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.691
_refine_diff_density_min         -2.696
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         4503
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0356P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0868
_reflns_number_gt                3303
_reflns_number_total             4503
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8009139_si_001_5.cif
_cod_data_source_block           apx374
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               4305984
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pu1 Pu 0.5000 0.18139(3) 0.7500 0.02257(11) Uani 1 2 d S . .
Pu2 Pu 0.0000 0.29425(3) 0.2500 0.02192(11) Uani 1 2 d S . .
Cl1 Cl 0.38451(17) 0.18900(16) 0.89057(14) 0.0375(5) Uani 1 1 d . . .
Cl2 Cl -0.00150(19) 0.30723(16) 0.43375(13) 0.0373(5) Uani 1 1 d . . .
Cl3 Cl 0.21762(17) 0.30868(17) 0.30130(15) 0.0396(5) Uani 1 1 d . . .
Cl4 Cl 0.0000 0.0666(2) 0.2500 0.0394(7) Uani 1 2 d S . .
O1 O 0.3224(4) 0.1133(5) 0.6373(4) 0.0375(13) Uani 1 1 d . . .
O2 O 0.4010(4) 0.3593(5) 0.6634(4) 0.0423(14) Uani 1 1 d . . .
O3 O 0.5000 -0.0382(6) 0.7500 0.0296(16) Uani 1 2 d S . .
O4 O 0.0000 0.5108(5) 0.2500 0.0275(16) Uani 1 2 d S . .
C1 C 0.2956(7) 0.1271(9) 0.5320(6) 0.060(3) Uani 1 1 d . . .
H1A H 0.3629 0.1173 0.5073 0.072 Uiso 1 1 calc R . .
H1B H 0.2640 0.2059 0.5131 0.072 Uiso 1 1 calc R . .
C2 C 0.2104(7) 0.0314(7) 0.4906(6) 0.045(2) Uani 1 1 d . . .
H2A H 0.1601 0.0565 0.4285 0.054 Uiso 1 1 calc R . .
H2B H 0.2472 -0.0428 0.4802 0.054 Uiso 1 1 calc R . .
C3 C 0.1482(8) 0.0180(9) 0.5694(6) 0.062(3) Uani 1 1 d . . .
H3A H 0.1155 -0.0615 0.5678 0.075 Uiso 1 1 calc R . .
H3B H 0.0881 0.0769 0.5616 0.075 Uiso 1 1 calc R . .
C4 C 0.2363(6) 0.0378(7) 0.6644(5) 0.0391(19) Uani 1 1 d . . .
H4A H 0.2039 0.0777 0.7129 0.047 Uiso 1 1 calc R . .
H4B H 0.2688 -0.0378 0.6919 0.047 Uiso 1 1 calc R . .
C5 C 0.2904(8) 0.3990(10) 0.6725(8) 0.077(4) Uani 1 1 d . . .
H5A H 0.2962 0.4357 0.7367 0.092 Uiso 1 1 calc R . .
H5B H 0.2386 0.3317 0.6654 0.092 Uiso 1 1 calc R . .
C6 C 0.2506(8) 0.4854(9) 0.5939(7) 0.062(3) Uani 1 1 d . . .
H6A H 0.1805 0.4577 0.5502 0.075 Uiso 1 1 calc R . .
H6B H 0.2364 0.5617 0.6218 0.075 Uiso 1 1 calc R . .
C7 C 0.3366(9) 0.4991(8) 0.5389(7) 0.059(3) Uani 1 1 d . . .
H7A H 0.3519 0.5833 0.5308 0.071 Uiso 1 1 calc R . .
H7B H 0.3117 0.4629 0.4738 0.071 Uiso 1 1 calc R . .
C8 C 0.4373(9) 0.4391(8) 0.5963(10) 0.091(4) Uani 1 1 d . . .
H8A H 0.4737 0.3945 0.5528 0.109 Uiso 1 1 calc R . .
H8B H 0.4908 0.4972 0.6328 0.109 Uiso 1 1 calc R . .
C9 C 0.5098(7) -0.1134(7) 0.6669(6) 0.047(2) Uani 1 1 d . . .
H9A H 0.5864 -0.1118 0.6584 0.056 Uiso 1 1 calc R . .
H9B H 0.4583 -0.0868 0.6060 0.056 Uiso 1 1 calc R . .
C10 C 0.4795(10) -0.2353(8) 0.6940(8) 0.086(4) Uani 1 1 d . . .
H10A H 0.5178 -0.2963 0.6647 0.104 Uiso 1 1 calc R . .
H10B H 0.3985 -0.2485 0.6732 0.104 Uiso 1 1 calc R . .
C11 C 0.0647(7) 0.5861(6) 0.3315(5) 0.0358(18) Uani 1 1 d . . .
H11A H 0.1453 0.5808 0.3362 0.043 Uiso 1 1 calc R . .
H11B H 0.0504 0.5625 0.3943 0.043 Uiso 1 1 calc R . .
C12 C 0.0213(9) 0.7106(7) 0.3030(6) 0.052(3) Uani 1 1 d . . .
H12A H -0.0385 0.7308 0.3350 0.063 Uiso 1 1 calc R . .
H12B H 0.0818 0.7687 0.3227 0.063 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
Pu Pu -9.4100 4.3056 '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
_geom_angle_publ_flag
O3 Pu1 O1 72.02(12) . . ?
O3 Pu1 O1 72.02(12) . 2_656 ?
O1 Pu1 O1 144.0(2) . 2_656 ?
O3 Pu1 O2 143.28(13) . 2_656 ?
O1 Pu1 O2 143.57(18) . 2_656 ?
O1 Pu1 O2 71.96(17) 2_656 2_656 ?
O3 Pu1 O2 143.28(13) . . ?
O1 Pu1 O2 71.96(17) . . ?
O1 Pu1 O2 143.57(18) 2_656 . ?
O2 Pu1 O2 73.4(3) 2_656 . ?
O3 Pu1 Cl1 91.82(4) . 2_656 ?
O1 Pu1 Cl1 94.69(13) . 2_656 ?
O1 Pu1 Cl1 86.43(13) 2_656 2_656 ?
O2 Pu1 Cl1 92.84(13) 2_656 2_656 ?
O2 Pu1 Cl1 84.24(13) . 2_656 ?
O3 Pu1 Cl1 91.82(4) . . ?
O1 Pu1 Cl1 86.43(13) . . ?
O1 Pu1 Cl1 94.69(13) 2_656 . ?
O2 Pu1 Cl1 84.24(13) 2_656 . ?
O2 Pu1 Cl1 92.84(13) . . ?
Cl1 Pu1 Cl1 176.36(8) 2_656 . ?
O4 Pu2 Cl4 180.0 . . ?
O4 Pu2 Cl2 86.76(4) . 2 ?
Cl4 Pu2 Cl2 93.24(4) . 2 ?
O4 Pu2 Cl2 86.76(4) . . ?
Cl4 Pu2 Cl2 93.24(4) . . ?
Cl2 Pu2 Cl2 173.53(8) 2 . ?
O4 Pu2 Cl3 86.42(4) . . ?
Cl4 Pu2 Cl3 93.58(4) . . ?
Cl2 Pu2 Cl3 90.83(7) 2 . ?
Cl2 Pu2 Cl3 88.77(7) . . ?
O4 Pu2 Cl3 86.42(4) . 2 ?
Cl4 Pu2 Cl3 93.58(4) . 2 ?
Cl2 Pu2 Cl3 88.77(7) 2 2 ?
Cl2 Pu2 Cl3 90.83(7) . 2 ?
Cl3 Pu2 Cl3 172.83(8) . 2 ?
C1 O1 C4 109.1(5) . . ?
C1 O1 Pu1 124.4(4) . . ?
C4 O1 Pu1 125.9(4) . . ?
C8 O2 C5 107.9(6) . . ?
C8 O2 Pu1 128.5(5) . . ?
C5 O2 Pu1 123.6(5) . . ?
C9 O3 C9 109.6(8) . 2_656 ?
C9 O3 Pu1 125.2(4) . . ?
C9 O3 Pu1 125.2(4) 2_656 . ?
C11 O4 C11 110.5(7) . 2 ?
C11 O4 Pu2 124.8(4) . . ?
C11 O4 Pu2 124.8(4) 2 . ?
O1 C1 C2 106.2(7) . . ?
C3 C2 C1 102.6(7) . . ?
C2 C3 C4 104.5(7) . . ?
O1 C4 C3 105.1(6) . . ?
O2 C5 C6 106.4(7) . . ?
C7 C6 C5 108.5(8) . . ?
C6 C7 C8 106.5(8) . . ?
O2 C8 C7 106.8(8) . . ?
O3 C9 C10 104.7(7) . . ?
C9 C10 C10 102.8(6) . 2_656 ?
O4 C11 C12 103.7(6) . . ?
C12 C12 C11 106.6(5) 2 . ?
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
Pu1 O3 2.451(6) . ?
Pu1 O1 2.462(5) . ?
Pu1 O1 2.462(5) 2_656 ?
Pu1 O2 2.478(5) 2_656 ?
Pu1 O2 2.478(5) . ?
Pu1 Cl1 2.6771(19) 2_656 ?
Pu1 Cl1 2.6771(19) . ?
Pu2 O4 2.417(6) . ?
Pu2 Cl4 2.541(3) . ?
Pu2 Cl2 2.5664(18) 2 ?
Pu2 Cl2 2.5664(18) . ?
Pu2 Cl3 2.577(2) . ?
Pu2 Cl3 2.577(2) 2 ?
O1 C1 1.431(8) . ?
O1 C4 1.465(8) . ?
O2 C8 1.437(10) . ?
O2 C5 1.453(9) . ?
O3 C9 1.458(8) . ?
O3 C9 1.458(8) 2_656 ?
O4 C11 1.475(7) . ?
O4 C11 1.475(7) 2 ?
C1 C2 1.502(11) . ?
C2 C3 1.486(11) . ?
C3 C4 1.502(10) . ?
C5 C6 1.450(11) . ?
C6 C7 1.449(12) . ?
C7 C8 1.454(12) . ?
C9 C10 1.483(12) . ?
C10 C10 1.52(2) 2_656 ?
C11 C12 1.505(10) . ?
C12 C12 1.439(16) 2 ?
