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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/4/12/63/4126320.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_4126320
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 N I 1+)2, (Np O2 Cl4)'
_chemical_formula_sum            'C10 H10 Cl4 I2 N2 Np O2'
_chemical_formula_weight         822.80
_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                 103.004(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.084(4)
_cell_length_b                   8.610(2)
_cell_length_c                   6.9394(18)
_cell_measurement_reflns_used    1573
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      54.334
_cell_measurement_theta_min      5.398
_cell_volume                     936.3(4)
_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      110(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Quazar'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2759
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         27.178
_diffrn_reflns_theta_min         2.599
_diffrn_source                   'moly microfocus'
_exptl_absorpt_coefficient_mu    9.419
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Krause et. al 2015'
_exptl_crystal_colour            Green-Yellow
_exptl_crystal_density_diffrn    2.918
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             734
_exptl_crystal_recrystallization_method 'Aqueous acidic (HCl) evaporation'
_exptl_crystal_size_max          0.045
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.794
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         1101
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0198
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0120P)²+2.1864P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0409
_refine_ls_wR_factor_ref         0.0425
_reflns_Friedel_coverage         0.000
_reflns_number_gt                979
_reflns_number_total             1101
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja7b05689_si_002.cif
_cod_data_source_block           Compound_8_110K
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4126320
_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   0.677
_shelx_estimated_absorpt_t_max   0.834
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
C1 C 0.6054(2) 0.1368(5) 0.6226(5) 0.0168(8) Uani 1 1 d . . .
H1 H 0.5904 0.2310 0.6775 0.020 Uiso 1 1 calc R U .
C2 C 0.6467(2) 0.1404(5) 0.4691(5) 0.0154(8) Uani 1 1 d . . .
H2 H 0.6600 0.2366 0.4160 0.018 Uiso 1 1 calc R U .
C3 C 0.6687(3) 0.0000 0.3929(7) 0.0134(11) Uani 1 2 d S T P
N1 N 0.5864(3) 0.0000 0.6942(6) 0.0158(10) Uani 1 2 d DS T P
O1 O 0.4681(2) 0.5000 0.2260(5) 0.0169(8) Uani 1 2 d S T P
Cl1 Cl 0.5000 0.80764(15) 0.0000 0.0156(3) Uani 1 2 d S T P
Cl2 Cl 0.33758(8) 0.5000 -0.19115(19) 0.0162(3) Uani 1 2 d S T P
I1 I 0.73737(2) 0.0000 0.17263(5) 0.01609(10) Uani 1 2 d S T P
Np1 Np 0.5000 0.5000 0.0000 0.01018(9) Uani 1 4 d S T P
HN1 H 0.556(4) 0.0000 0.784(8) 0.04(2) Uiso 1 2 d DS . P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Np Np -11.4937 4.1493 '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
N1 C1 C2 119.8(4) . .
N1 C1 H1 120.1 . .
C2 C1 H1 120.1 . .
C1 C2 C3 118.7(4) . .
C1 C2 H2 120.6 . .
C3 C2 H2 120.6 . .
C2 C3 C2 119.9(5) . 6
C2 C3 I1 120.0(2) . .
C2 C3 I1 120.0(2) 6 .
C1 N1 C1 123.0(5) . 6
C1 N1 HN1 118.3(4) . .
C1 N1 HN1 118.3(4) 6 .
O1 Np1 O1 180.0 5_665 .
O1 Np1 Cl1 90.0 5_665 .
O1 Np1 Cl1 90.0 . .
O1 Np1 Cl1 90.0 5_665 5_665
O1 Np1 Cl1 90.0 . 5_665
Cl1 Np1 Cl1 180.0 . 5_665
O1 Np1 Cl2 89.65(13) 5_665 5_665
O1 Np1 Cl2 90.35(13) . 5_665
Cl1 Np1 Cl2 90.0 . 5_665
Cl1 Np1 Cl2 90.0 5_665 5_665
O1 Np1 Cl2 90.35(13) 5_665 .
O1 Np1 Cl2 89.65(13) . .
Cl1 Np1 Cl2 90.0 . .
Cl1 Np1 Cl2 90.0 5_665 .
Cl2 Np1 Cl2 180.0 5_665 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.340(4) .
C1 C2 1.377(5) .
C1 H1 0.9500 .
C2 C3 1.396(5) .
C2 H2 0.9500 .
C3 C2 1.396(5) 6
C3 I1 2.078(5) .
N1 C1 1.340(4) 6
N1 HN1 0.88(2) .
O1 Np1 1.756(4) .
Cl1 Np1 2.6487(15) .
Cl2 Np1 2.6504(14) .
Np1 O1 1.756(4) 5_665
Np1 Cl1 2.6487(15) 5_665
Np1 Cl2 2.6504(14) 5_665
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C1 H1 O1 0.95 2.64 3.583(4) 170.7 5_666
C1 H1 Cl1 0.95 2.95 3.458(4) 114.9 5_666
C2 H2 Cl2 0.95 2.76 3.686(4) 165.7 5_665
N1 HN1 Cl1 0.88(2) 2.530(16) 3.241(4) 138.7(8) 1_546
N1 HN1 Cl1 0.88(2) 2.530(16) 3.241(4) 138.7(8) 5_666
C1 H1 O1 0.95 2.64 3.583(4) 170.7 5_666
C1 H1 Cl1 0.95 2.95 3.458(4) 114.9 5_666
C2 H2 Cl2 0.95 2.76 3.686(4) 165.7 5_665
N1 HN1 Cl1 0.88(2) 2.530(16) 3.241(4) 138.7(8) 1_546
N1 HN1 Cl1 0.88(2) 2.530(16) 3.241(4) 138.7(8) 5_666
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_4
N1 C1 C2 C3 -0.7(6) .
C1 C2 C3 C2 1.7(8) 6
C1 C2 C3 I1 -176.4(3) .
C2 C1 N1 C1 -0.3(8) 6
