#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:10:58 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179097 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/59/4305983.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_4305983
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            'C21 H37 I5 N O4 Pu'
_chemical_formula_weight         1244.02
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6162(13)
_cell_length_b                   22.066(2)
_cell_length_c                   11.8472(12)
_cell_measurement_temperature    141(2)
_cell_volume                     3298.1(6)
_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 0.957
_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  0.0488
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            34406
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.85
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.703
_exptl_absorpt_correction_T_max  0.8776
_exptl_absorpt_correction_T_min  0.5538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    2.505
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular slab'
_exptl_crystal_F_000             2244
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.029
_refine_diff_density_min         -1.705
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.606
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         4139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.606
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0355
_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)+(0.0294P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0948
_reflns_number_gt                2978
_reflns_number_total             4139
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8009139_si_001_4.cif
_cod_data_source_block           apx277a
_cod_database_code               4305983
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'
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 0.0000 0.197609(14) 0.2500 0.02659(10) Uani 1 2 d S . .
I1 I 0.01465(4) 0.19736(2) 0.50884(4) 0.04390(14) Uani 1 1 d . . .
I2 I 0.77602(4) 0.47659(2) 1.03998(5) 0.05769(17) Uani 1 1 d . . .
I3 I 1.0000 0.5000 1.0000 0.04567(18) Uani 1 2 d S . .
O1 O 0.1854(3) 0.1641(2) 0.2325(3) 0.0340(10) Uani 1 1 d . . .
O2 O -0.1154(4) 0.2888(2) 0.2590(3) 0.0400(11) Uani 1 1 d . . .
N1 N 0.0000 0.0800(3) 0.2500 0.0341(16) Uani 1 2 d S . .
C1 C 0.2411(6) 0.1251(4) 0.3086(7) 0.062(2) Uani 1 1 d . . .
H1A H 0.2317 0.1393 0.3855 0.074 Uiso 1 1 calc R . .
H1B H 0.2126 0.0844 0.3035 0.074 Uiso 1 1 calc R . .
C2 C 0.3451(7) 0.1245(8) 0.2825(11) 0.170(8) Uani 1 1 d . . .
H2A H 0.3683 0.0829 0.2725 0.204 Uiso 1 1 calc R . .
H2B H 0.3852 0.1418 0.3445 0.204 Uiso 1 1 calc R . .
C3 C 0.3671(5) 0.1590(3) 0.1789(7) 0.054(2) Uani 1 1 d . . .
H3A H 0.4010 0.1337 0.1225 0.064 Uiso 1 1 calc R . .
H3B H 0.4119 0.1937 0.1945 0.064 Uiso 1 1 calc R . .
C4 C 0.2597(5) 0.1785(3) 0.1410(6) 0.0399(15) Uani 1 1 d . . .
H4A H 0.2592 0.2217 0.1255 0.048 Uiso 1 1 calc R . .
H4B H 0.2398 0.1571 0.0726 0.048 Uiso 1 1 calc R . .
C5 C -0.1112(7) 0.3357(3) 0.3454(7) 0.063(2) Uani 1 1 d . . .
H5A H -0.0472 0.3596 0.3374 0.076 Uiso 1 1 calc R . .
H5B H -0.1117 0.3176 0.4200 0.076 Uiso 1 1 calc R . .
C6 C -0.2063(8) 0.3743(4) 0.3294(8) 0.084(3) Uani 1 1 d . . .
H6A H -0.1858 0.4147 0.3054 0.101 Uiso 1 1 calc R . .
H6B H -0.2459 0.3776 0.3994 0.101 Uiso 1 1 calc R . .
C7 C -0.2732(6) 0.3436(4) 0.2389(6) 0.056(2) Uani 1 1 d . . .
H7A H -0.3310 0.3209 0.2723 0.068 Uiso 1 1 calc R . .
H7B H -0.3020 0.3731 0.1865 0.068 Uiso 1 1 calc R . .
C8 C -0.1971(5) 0.3028(3) 0.1820(6) 0.0445(17) Uani 1 1 d . . .
H8A H -0.2326 0.2660 0.1581 0.053 Uiso 1 1 calc R . .
H8B H -0.1678 0.3226 0.1158 0.053 Uiso 1 1 calc R . .
C9 C 0.0395(6) 0.0472(3) 0.1640(7) 0.0485(18) Uani 1 1 d . . .
H9 H 0.0679 0.0674 0.1021 0.058 Uiso 1 1 calc R . .
C10 C 0.0394(6) -0.0157(3) 0.1645(8) 0.057(2) Uani 1 1 d . . .
H10 H 0.0679 -0.0363 0.1032 0.068 Uiso 1 1 calc R . .
C11 C 0.0000 -0.0471(6) 0.2500 0.059(3) Uani 1 2 d S . .
H11 H 0.0000 -0.0893 0.2500 0.071 Uiso 1 2 calc SR . .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
O O 0.0106 0.0060 '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
O1 Pu1 O1 145.1(2) . 3 ?
O1 Pu1 O2 71.50(15) . 3 ?
O1 Pu1 O2 143.40(15) 3 3 ?
O1 Pu1 O2 143.40(15) . . ?
O1 Pu1 O2 71.50(15) 3 . ?
O2 Pu1 O2 71.9(2) 3 . ?
O1 Pu1 N1 72.55(10) . . ?
O1 Pu1 N1 72.55(10) 3 . ?
O2 Pu1 N1 144.04(11) 3 . ?
O2 Pu1 N1 144.04(11) . . ?
O1 Pu1 I1 91.50(9) . . ?
O1 Pu1 I1 88.44(9) 3 . ?
O2 Pu1 I1 90.51(9) 3 . ?
O2 Pu1 I1 89.66(9) . . ?
N1 Pu1 I1 89.896(10) . . ?
O1 Pu1 I1 88.44(9) . 3 ?
O1 Pu1 I1 91.50(9) 3 3 ?
O2 Pu1 I1 89.66(9) 3 3 ?
O2 Pu1 I1 90.51(9) . 3 ?
N1 Pu1 I1 89.896(10) . 3 ?
I1 Pu1 I1 179.79(2) . 3 ?
I2 I3 I2 180.0 5_767 . ?
C1 O1 C4 106.4(5) . . ?
C1 O1 Pu1 126.4(4) . . ?
C4 O1 Pu1 127.2(3) . . ?
C8 O2 C5 109.0(5) . . ?
C8 O2 Pu1 125.3(4) . . ?
C5 O2 Pu1 125.7(4) . . ?
C9 N1 C9 114.9(8) . 3 ?
C9 N1 Pu1 122.5(4) . . ?
C9 N1 Pu1 122.5(4) 3 . ?
C2 C1 O1 109.8(7) . . ?
C1 C2 C3 111.6(7) . . ?
C2 C3 C4 103.3(6) . . ?
O1 C4 C3 107.1(5) . . ?
O2 C5 C6 106.8(6) . . ?
C5 C6 C7 106.4(6) . . ?
C8 C7 C6 103.5(6) . . ?
O2 C8 C7 108.2(6) . . ?
N1 C9 C10 122.3(7) . . ?
C11 C10 C9 121.8(9) . . ?
C10 C11 C10 116.8(12) 3 . ?
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 O1 2.462(4) . ?
Pu1 O1 2.462(4) 3 ?
Pu1 O2 2.486(4) 3 ?
Pu1 O2 2.486(4) . ?
Pu1 N1 2.596(7) . ?
Pu1 I1 3.0721(5) . ?
Pu1 I1 3.0721(5) 3 ?
I2 I3 2.9113(6) . ?
I3 I2 2.9113(6) 5_767 ?
O1 C1 1.431(8) . ?
O1 C4 1.468(7) . ?
O2 C8 1.411(7) . ?
O2 C5 1.457(8) . ?
N1 C9 1.345(8) . ?
N1 C9 1.345(8) 3 ?
C1 C2 1.348(11) . ?
C2 C3 1.471(11) . ?
C3 C4 1.490(9) . ?
C5 C6 1.484(11) . ?
C6 C7 1.524(12) . ?
C7 C8 1.478(10) . ?
C9 C10 1.387(10) . ?
C10 C11 1.325(10) . ?
C11 C10 1.325(10) 3 ?
