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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/4/12/63/4126312.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_4126312
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 Br N 1+)2, (Np O2 Cl4 2-)'
_chemical_formula_sum            'C10 H10 Br2 Cl4 N2 Np O2'
_chemical_formula_weight         728.82
_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   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 102.023(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.9996(11)
_cell_length_b                   8.6659(6)
_cell_length_c                   6.8488(5)
_cell_measurement_reflns_used    9339
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      55.805
_cell_measurement_theta_min      4.799
_cell_volume                     928.76(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 0.999
_diffrn_measured_fraction_theta_max 0.993
_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  0.0361
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            33516
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         27.992
_diffrn_reflns_theta_min         2.399
_diffrn_source                   'Silver microfocus'
_exptl_absorpt_coefficient_mu    9.067
_exptl_absorpt_correction_T_max  0.390
_exptl_absorpt_correction_T_min  0.146
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Krause et. al 2015'
_exptl_crystal_colour            Yellow-Green
_exptl_crystal_density_diffrn    2.606
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             662
_exptl_crystal_recrystallization_method 'Acidic (HCl) aqueous evaporation'
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.183
_exptl_crystal_size_min          0.128
_exptl_transmission_factor_max   0.7456
_exptl_transmission_factor_min   0.3103
_refine_diff_density_max         1.168
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       0.0156(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   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     59
_refine_ls_number_reflns         2393
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0166
_refine_ls_R_factor_gt           0.0165
_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)+(0.0127P)²+1.3918P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0332
_refine_ls_wR_factor_ref         0.0333
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2386
_reflns_number_total             2393
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja7b05689_si_002.cif
_cod_data_source_block           Compound_7
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4126312
_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'
'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 0.89003(15) 0.3653(3) 0.3784(3) 0.0449(4) Uani 1 1 d . . .
H1 H 0.9046 0.2736 0.3232 0.054 Uiso 1 1 calc R U .
C2 C 0.84989(13) 0.3613(3) 0.5361(3) 0.0411(4) Uani 1 1 d . . .
H2 H 0.8372 0.2679 0.5902 0.049 Uiso 1 1 calc R U .
C3 C 0.82865(16) 0.5000 0.6129(4) 0.0359(5) Uani 1 2 d S T P
N1 N 0.90832(17) 0.5000 0.3036(4) 0.0431(5) Uani 1 2 d S T P
HN1 H 0.9329 0.5000 0.2032 0.052 Uiso 1 2 calc R U P
O1 O 0.53299(14) 0.5000 -0.2284(3) 0.0383(4) Uani 1 2 d S T P
Cl1 Cl 0.5000 0.80639(6) 0.0000 0.03763(12) Uani 1 2 d S T P
Cl2 Cl 0.66201(4) 0.5000 0.18813(12) 0.04324(14) Uani 1 2 d S T P
Br1 Br 0.76769(2) 0.5000 0.81786(5) 0.05551(9) Uani 1 2 d S T P
Np1 Np 0.5000 0.5000 0.0000 0.02227(4) Uani 1 4 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'
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'
Cl Cl 0.0998 0.0984 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br 0.1811 1.6452 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Np Np -6.9995 9.5876 '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 120.2(2) . .
N1 C1 H1 119.9 . .
C2 C1 H1 119.9 . .
C1 C2 C3 118.2(2) . .
C1 C2 H2 120.9 . .
C3 C2 H2 120.9 . .
C2 C3 C2 120.8(3) 6_565 .
C2 C3 Br1 119.60(13) 6_565 .
C2 C3 Br1 119.60(13) . .
C1 N1 C1 122.5(3) 6_565 .
C1 N1 HN1 118.8 6_565 .
C1 N1 HN1 118.8 . .
O1 Np1 O1 180.0 5_665 .
O1 Np1 Cl2 89.31(8) 5_665 5_665
O1 Np1 Cl2 90.69(8) . 5_665
O1 Np1 Cl2 90.69(8) 5_665 .
O1 Np1 Cl2 89.31(8) . .
Cl2 Np1 Cl2 180.0 5_665 .
O1 Np1 Cl1 90.0 5_665 .
O1 Np1 Cl1 90.0 . .
Cl2 Np1 Cl1 90.0 5_665 .
Cl2 Np1 Cl1 90.0 . .
O1 Np1 Cl1 90.0 5_665 5_665
O1 Np1 Cl1 90.0 . 5_665
Cl2 Np1 Cl1 90.0 5_665 5_665
Cl2 Np1 Cl1 90.0 . 5_665
Cl1 Np1 Cl1 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 1.332(3) .
C1 C2 1.367(3) .
C1 H1 0.9300 .
C2 C3 1.383(3) .
C2 H2 0.9300 .
C3 C2 1.383(3) 6_565
C3 Br1 1.869(3) .
N1 C1 1.332(3) 6_565
N1 HN1 0.8600 .
O1 Np1 1.7520(18) .
Cl1 Np1 2.6552(6) .
Cl2 Np1 2.6434(7) .
Np1 O1 1.7520(18) 5_665
Np1 Cl2 2.6434(7) 5_665
Np1 Cl1 2.6552(6) 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 Cl1 0.93 2.95 3.460(2) 115.8 3_545
C2 H2 Cl2 0.93 2.77 3.682(2) 166.1 7_656
N1 HN1 Cl1 0.86 2.56 3.250(2) 138.5 3_545
N1 HN1 Cl1 0.86 2.56 3.250(2) 138.5 7_665
C1 H1 Cl1 0.93 2.95 3.460(2) 115.8 3_545
C2 H2 Cl2 0.93 2.77 3.682(2) 166.1 7_656
N1 HN1 Cl1 0.86 2.56 3.250(2) 138.5 3_545
N1 HN1 Cl1 0.86 2.56 3.250(2) 138.5 7_665
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 0.5(3) .
C1 C2 C3 C2 -2.0(4) 6_565
C1 C2 C3 Br1 176.20(17) .
C2 C1 N1 C1 1.0(5) 6_565
