#------------------------------------------------------------------------------
#$Date: 2017-07-27 01:34:31 +0300 (Thu, 27 Jul 2017) $
#$Revision: 199346 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/63/4126317.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_4126317
loop_
_publ_author_name
'Surbella, Robert G.'
'Ducati, Lucas Colucci'
'Pellegrini, Kristi L.'
'McNamara, Bruce K.'
'Autschbach, Jochen'
'Schwantes, Jon Michael'
'Cahill, Christopher L.'
_publ_section_title
;
 Transuranic Hybrid Materials: Crystallographic and Computational Metrics
 of Supramolecular Assembly.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b05689
_journal_year                    2017
_chemical_formula_moiety         '(C5 H5 I N 1+)2, (Pu O2 Cl4 2-)'
_chemical_formula_sum            'C10 H10 Cl4 I2 N2 O2 Pu'
_chemical_formula_weight         827.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      12
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 102.267(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.4644(11)
_cell_length_b                   8.7019(5)
_cell_length_c                   6.8794(5)
_cell_measurement_reflns_used    6942
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      47.476
_cell_measurement_theta_min      4.782
_cell_volume                     963.12(11)
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_collection       'APEX, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_molecular_graphics    'WINGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR92 (Gualardi, 1994)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Venture, Photon CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            9893
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        23.740
_diffrn_reflns_theta_max         23.740
_diffrn_reflns_theta_min         2.391
_diffrn_source                   'Silver microfocus'
_exptl_absorpt_coefficient_mu    6.725
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.5206
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Krause et. al 2015'
_exptl_crystal_colour            Yellow-Orange
_exptl_crystal_density_diffrn    2.854
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             736
_exptl_crystal_recrystallization_method 'Acidic (HCl) aqueous evaporation'
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.122
_refine_diff_density_max         0.998
_refine_diff_density_min         -1.332
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       0.0059(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     59
_refine_ls_number_reflns         1570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0210
_refine_ls_R_factor_gt           0.0202
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0176P)²+5.0468P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0512
_refine_ls_wR_factor_ref         0.0517
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1542
_reflns_number_total             1570
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja7b05689_si_002.cif
_cod_data_source_block           Compound_12
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4126317
_shelx_shelxl_version_number     2014/7
_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.
;
_shelx_estimated_absorpt_t_min   0.341
_shelx_estimated_absorpt_t_max   0.494
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
I1 I 0.23850(3) 0.5000 0.17173(6) 0.04886(12) Uani 1 2 d S T P
N1 N 0.0871(3) 0.5000 0.6936(7) 0.0451(11) Uani 1 2 d S T P
HN1 H 0.0580 0.5000 0.7850 0.054 Uiso 1 2 d R U P
C1 C 0.1064(3) 0.3664(6) 0.6218(7) 0.0478(10) Uani 1 1 d . . .
H1 H 0.0915 0.2750 0.6752 0.057 Uiso 1 1 calc R U .
C2 C 0.1481(3) 0.3625(5) 0.4690(7) 0.0442(9) Uani 1 1 d . . .
H2 H 0.1613 0.2693 0.4172 0.053 Uiso 1 1 calc R U .
C3 C 0.1703(3) 0.5000 0.3936(8) 0.0368(11) Uani 1 2 d S T P
Pu1 Pu 0.0000 0.0000 0.0000 0.02066(9) Uani 1 4 d S T P
Cl1 Cl 0.0000 0.30537(14) 0.0000 0.0418(3) Uani 1 2 d S T P
Cl2 Cl 0.15790(9) 0.0000 0.1924(2) 0.0447(3) Uani 1 2 d S T P
O1 O -0.0319(3) 0.0000 0.2259(6) 0.0407(8) Uani 1 2 d S T P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 '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 0.0998 0.0984 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.8919 1.1868 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pu Pu -13.5905 6.9468 '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
C1 N1 C1 122.2(5) . 6_565
C1 N1 HN1 118.8 . .
C1 N1 HN1 118.8 6_565 .
N1 C1 C2 120.3(4) . .
N1 C1 H1 119.9 . .
C2 C1 H1 119.9 . .
C1 C2 C3 118.7(4) . .
C1 C2 H2 120.6 . .
C3 C2 H2 120.6 . .
C2 C3 C2 119.7(5) 6_565 .
C2 C3 I1 120.1(3) 6_565 .
C2 C3 I1 120.1(3) . .
O1 Pu1 O1 180.0(3) 5 .
O1 Pu1 Cl2 90.24(15) 5 5
O1 Pu1 Cl2 89.76(15) . 5
O1 Pu1 Cl2 89.76(15) 5 .
O1 Pu1 Cl2 90.24(15) . .
Cl2 Pu1 Cl2 180.00(3) 5 .
O1 Pu1 Cl1 90.0 5 .
O1 Pu1 Cl1 90.0 . .
Cl2 Pu1 Cl1 90.0 5 .
Cl2 Pu1 Cl1 90.0 . .
O1 Pu1 Cl1 90.0 5 5
O1 Pu1 Cl1 90.0 . 5
Cl2 Pu1 Cl1 90.0 5 5
Cl2 Pu1 Cl1 90.0 . 5
Cl1 Pu1 Cl1 180.0 . 5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 C3 2.078(5) .
N1 C1 1.328(5) .
N1 C1 1.328(5) 6_565
N1 HN1 0.8677 .
C1 C2 1.373(6) .
C1 H1 0.9300 .
C2 C3 1.383(5) .
C2 H2 0.9300 .
C3 C2 1.383(5) 6_565
Pu1 O1 1.743(4) 5
Pu1 O1 1.743(4) .
Pu1 Cl2 2.6549(14) 5
Pu1 Cl2 2.6549(14) .
Pu1 Cl1 2.6573(12) .
Pu1 Cl1 2.6573(12) 5
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C1 N1 C1 C2 0.4(9) 6_565 .
N1 C1 C2 C3 0.7(7) . .
C1 C2 C3 C2 -1.8(9) . 6_565
C1 C2 C3 I1 177.1(3) . .
