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#$Date: 2017-07-27 01:34:31 +0300 (Thu, 27 Jul 2017) $
#$Revision: 199346 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/63/4126314.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_4126314
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 H6 N 1+)2, (Pu O2 Cl4 2-)'
_chemical_formula_sum            'C10 H12 Cl4 N2 O2 Pu'
_chemical_formula_weight         576.02
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                77.9360(10)
_cell_angle_beta                 71.7730(10)
_cell_angle_gamma                75.4320(10)
_cell_formula_units_Z            2
_cell_length_a                   7.7417(4)
_cell_length_b                   10.3137(5)
_cell_length_c                   11.2637(6)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      59.232
_cell_measurement_theta_min      5.901
_cell_volume                     818.42(7)
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture, Photon CCD'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0152
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            31093
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.665
_diffrn_reflns_theta_min         2.950
_diffrn_source                   'Fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.677
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5315
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Krause et. al 2015'
_exptl_crystal_colour            Yellow-Orange
_exptl_crystal_density_diffrn    2.337
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             528
_exptl_crystal_recrystallization_method 'Acidic (HCl) aqueous evaporation'
_exptl_crystal_size_max          0.291
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         4630
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0208
_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)+(0.0229P)²+0.5398P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0467
_refine_ls_wR_factor_ref         0.0512
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3577
_reflns_number_total             4630
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja7b05689_si_002.cif
_cod_data_source_block           Compound_9
_cod_database_code               4126314
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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
Pu1 Pu 0.5000 0.0000 1.0000 0.04264(5) Uani 1 2 d S . P
Cl1 Cl 0.33417(14) 0.16858(10) 0.83752(8) 0.0631(2) Uani 1 1 d . . .
Cl2 Cl 0.82928(15) 0.03284(12) 0.84187(11) 0.0752(3) Uani 1 1 d . . .
O1 O 0.5053(4) -0.1350(2) 0.9286(2) 0.0607(6) Uani 1 1 d . . .
Pu2 Pu 0.0000 0.5000 0.5000 0.04211(5) Uani 1 2 d S . P
Cl3 Cl 0.32775(14) 0.55554(11) 0.35627(10) 0.0657(2) Uani 1 1 d . . .
Cl4 Cl 0.05312(15) 0.30239(10) 0.36780(9) 0.0665(2) Uani 1 1 d . . .
O2 O 0.1072(4) 0.3882(2) 0.6051(2) 0.0613(6) Uani 1 1 d . . .
N1 N 0.5678(5) 0.2354(4) 0.4885(4) 0.0818(11) Uani 1 1 d . . .
HN1 H 0.5076 0.3137 0.5083 0.098 Uiso 1 1 d R U .
C1 C 0.5673(6) 0.1986(4) 0.3781(4) 0.0655(10) Uani 1 1 d . . .
H1 H 0.4998 0.2562 0.3256 0.079 Uiso 1 1 calc R U .
C2 C 0.6681(6) 0.0755(5) 0.3477(3) 0.0664(11) Uani 1 1 d . . .
H2 H 0.6723 0.0484 0.2730 0.080 Uiso 1 1 calc R U .
C3 C 0.7637(5) -0.0084(4) 0.4282(4) 0.0637(10) Uani 1 1 d . . .
H3 H 0.8338 -0.0926 0.4087 0.076 Uiso 1 1 calc R U .
C4 C 0.7539(5) 0.0342(4) 0.5370(4) 0.0608(9) Uani 1 1 d . . .
H4 H 0.8159 -0.0221 0.5933 0.073 Uiso 1 1 calc R U .
C5 C 0.6584(5) 0.1533(4) 0.5632(3) 0.0502(7) Uani 1 1 d . . .
H5 H 0.6550 0.1803 0.6378 0.060 Uiso 1 1 calc R U .
N2 N 0.8989(6) 0.2700(4) 0.0052(4) 0.0834(12) Uani 1 1 d . . .
HN2 H 0.9541 0.1883 -0.0062 0.100 Uiso 1 1 d R U .
C6 C 0.8896(6) 0.3138(5) 0.1095(4) 0.0684(10) Uani 1 1 d . . .
H6 H 0.9433 0.2563 0.1695 0.082 Uiso 1 1 calc R U .
C7 C 0.8039(6) 0.4401(5) 0.1297(4) 0.0710(11) Uani 1 1 d . . .
H7 H 0.7961 0.4699 0.2040 0.085 Uiso 1 1 calc R U .
C8 C 0.7279(6) 0.5254(4) 0.0409(5) 0.0741(12) Uani 1 1 d . . .
H8 H 0.6679 0.6137 0.0537 0.089 Uiso 1 1 calc R U .
C9 C 0.7417(7) 0.4783(5) -0.0682(4) 0.0759(12) Uani 1 1 d . . .
H9 H 0.6938 0.5357 -0.1309 0.091 Uiso 1 1 calc R U .
C10 C 0.8232(7) 0.3514(5) -0.0840(4) 0.0769(12) Uani 1 1 d . . .
H10 H 0.8283 0.3184 -0.1560 0.092 Uiso 1 1 calc R U .
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'
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'
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
O1 Pu1 O1 180.00(17) . 2_657
O1 Pu1 Cl1 89.93(9) . .
O1 Pu1 Cl1 90.07(9) 2_657 .
O1 Pu1 Cl1 90.07(9) . 2_657
O1 Pu1 Cl1 89.93(9) 2_657 2_657
Cl1 Pu1 Cl1 180.0 . 2_657
O1 Pu1 Cl2 89.67(9) . 2_657
O1 Pu1 Cl2 90.33(9) 2_657 2_657
Cl1 Pu1 Cl2 90.49(4) . 2_657
Cl1 Pu1 Cl2 89.51(4) 2_657 2_657
O1 Pu1 Cl2 90.33(9) . .
O1 Pu1 Cl2 89.67(9) 2_657 .
Cl1 Pu1 Cl2 89.51(4) . .
Cl1 Pu1 Cl2 90.49(4) 2_657 .
Cl2 Pu1 Cl2 180.0 2_657 .
O2 Pu2 O2 180.0 . 2_566
O2 Pu2 Cl4 89.95(9) . .
O2 Pu2 Cl4 90.05(9) 2_566 .
O2 Pu2 Cl4 90.05(9) . 2_566
O2 Pu2 Cl4 89.95(9) 2_566 2_566
Cl4 Pu2 Cl4 180.0 . 2_566
O2 Pu2 Cl3 90.46(10) . .
O2 Pu2 Cl3 89.54(10) 2_566 .
Cl4 Pu2 Cl3 88.65(3) . .
Cl4 Pu2 Cl3 91.35(3) 2_566 .
O2 Pu2 Cl3 89.54(10) . 2_566
O2 Pu2 Cl3 90.46(10) 2_566 2_566
Cl4 Pu2 Cl3 91.35(3) . 2_566
Cl4 Pu2 Cl3 88.65(3) 2_566 2_566
Cl3 Pu2 Cl3 180.00(3) . 2_566
C5 N1 C1 120.7(4) . .
C5 N1 HN1 119.6 . .
C1 N1 HN1 119.6 . .
C2 C1 N1 118.2(4) . .
C2 C1 H1 120.9 . .
N1 C1 H1 120.9 . .
C1 C2 C3 119.6(4) . .
C1 C2 H2 120.2 . .
C3 C2 H2 120.2 . .
C4 C3 C2 118.7(4) . .
C4 C3 H3 120.7 . .
C2 C3 H3 120.7 . .
C5 C4 C3 120.6(4) . .
C5 C4 H4 119.7 . .
C3 C4 H4 119.7 . .
N1 C5 C4 122.2(4) . .
N1 C5 H5 118.9 . .
C4 C5 H5 118.9 . .
C6 N2 C10 121.1(4) . .
C6 N2 HN2 119.4 . .
C10 N2 HN2 119.4 . .
N2 C6 C7 120.5(4) . .
N2 C6 H6 119.7 . .
C7 C6 H6 119.7 . .
C6 C7 C8 119.8(4) . .
C6 C7 H7 120.1 . .
C8 C7 H7 120.1 . .
C7 C8 C9 118.7(4) . .
C7 C8 H8 120.7 . .
C9 C8 H8 120.7 . .
C10 C9 C8 120.1(4) . .
C10 C9 H9 119.9 . .
C8 C9 H9 119.9 . .
C9 C10 N2 119.7(4) . .
C9 C10 H10 120.2 . .
N2 C10 H10 120.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pu1 O1 1.734(2) .
Pu1 O1 1.734(2) 2_657
Pu1 Cl1 2.6528(10) .
Pu1 Cl1 2.6528(10) 2_657
Pu1 Cl2 2.6696(10) 2_657
Pu1 Cl2 2.6697(10) .
Pu2 O2 1.728(2) .
Pu2 O2 1.728(2) 2_566
Pu2 Cl4 2.6465(9) .
Pu2 Cl4 2.6465(9) 2_566
Pu2 Cl3 2.6760(10) .
Pu2 Cl3 2.6760(10) 2_566
N1 C5 1.300(6) .
N1 C1 1.376(6) .
N1 HN1 0.8602 .
C1 C2 1.361(6) .
C1 H1 0.9300 .
C2 C3 1.374(6) .
C2 H2 0.9300 .
C3 C4 1.361(6) .
C3 H3 0.9300 .
C4 C5 1.304(5) .
C4 H4 0.9300 .
C5 H5 0.9300 .
N2 C6 1.321(6) .
N2 C10 1.351(7) .
N2 HN2 0.8596 .
C6 C7 1.335(6) .
C6 H6 0.9300 .
C7 C8 1.364(6) .
C7 H7 0.9300 .
C8 C9 1.378(6) .
C8 H8 0.9300 .
C9 C10 1.325(7) .
C9 H9 0.9300 .
C10 H10 0.9300 .
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
C5 N1 C1 C2 -1.8(6)
N1 C1 C2 C3 1.1(6)
C1 C2 C3 C4 0.3(6)
C2 C3 C4 C5 -1.2(6)
C1 N1 C5 C4 0.9(6)
C3 C4 C5 N1 0.7(6)
C10 N2 C6 C7 0.3(7)
N2 C6 C7 C8 -1.1(7)
C6 C7 C8 C9 0.1(7)
C7 C8 C9 C10 1.8(7)
C8 C9 C10 N2 -2.5(7)
C6 N2 C10 C9 1.5(7)
