#------------------------------------------------------------------------------
#$Date: 2017-07-27 01:34:31 +0300 (Thu, 27 Jul 2017) $
#$Revision: 199346 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/63/4126319.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_4126319
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 Br 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   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 102.3490(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.715(2)
_cell_length_b                   8.6156(11)
_cell_length_c                   6.8740(9)
_cell_measurement_reflns_used    4014
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      57.976
_cell_measurement_theta_min      5.307
_cell_volume                     909.2(2)
_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 1.000
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'omega scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5741
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.290
_diffrn_reflns_theta_min         2.654
_diffrn_source                   'moly microfocus'
_diffrn_source_type              'Bruker Quazar'
_exptl_absorpt_coefficient_mu    10.699
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6038
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Krause et. al 2015'
_exptl_crystal_colour            Green-yellow
_exptl_crystal_density_diffrn    2.662
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             662
_exptl_crystal_recrystallization_method 'Aqueous acidic (HCl) evaporation'
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         1240
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0142
_refine_ls_R_factor_gt           0.0133
_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)+(0.0084P)²+1.6095P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0292
_refine_ls_wR_factor_ref         0.0297
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1197
_reflns_number_total             1240
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja7b05689_si_002.cif
_cod_data_source_block           Compound_7_110K
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4126319
_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   0.674
_shelx_estimated_absorpt_t_max   0.776
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
Np1 Np 0.5000 0.5000 1.0000 0.01052(5) Uani 1 4 d S T P
Br1 Br 0.26801(2) 0.0000 0.82090(4) 0.02172(8) Uani 1 2 d S T P
Cl2 Cl 0.5000 0.19221(8) 1.0000 0.01574(14) Uani 1 2 d S T P
Cl1 Cl 0.33468(4) 0.5000 0.81109(11) 0.01733(14) Uani 1 2 d S T P
O1 O 0.53333(14) 0.5000 0.7717(3) 0.0174(4) Uani 1 2 d S T P
N1 N 0.40901(17) 0.0000 0.3040(4) 0.0174(5) Uani 1 2 d DS T P
C1 C 0.39076(14) 0.1367(2) 0.3788(3) 0.0181(4) Uani 1 1 d . . .
H1 H 0.4055 0.2308 0.3219 0.022 Uiso 1 1 calc R U .
C3 C 0.32934(18) 0.0000 0.6155(4) 0.0158(6) Uani 1 2 d S T P
C2 C 0.35083(13) 0.1404(3) 0.5377(3) 0.0177(4) Uani 1 1 d . . .
H2 H 0.3381 0.2363 0.5934 0.021 Uiso 1 1 calc R U .
HN1 H 0.432(2) 0.0000 0.198(4) 0.035(11) 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'
Br Br -0.2901 2.4595 '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
O1 Np1 O1 180.00(4) 5_667 .
O1 Np1 Cl1 90.61(7) 5_667 5_667
O1 Np1 Cl1 89.39(7) . 5_667
O1 Np1 Cl1 89.39(7) 5_667 .
O1 Np1 Cl1 90.61(7) . .
Cl1 Np1 Cl1 180.0 5_667 .
O1 Np1 Cl2 90.0 5_667 5_667
O1 Np1 Cl2 90.0 . 5_667
Cl1 Np1 Cl2 90.0 5_667 5_667
Cl1 Np1 Cl2 90.0 . 5_667
O1 Np1 Cl2 90.0 5_667 .
O1 Np1 Cl2 90.0 . .
Cl1 Np1 Cl2 90.0 5_667 .
Cl1 Np1 Cl2 90.0 . .
Cl2 Np1 Cl2 180.0 5_667 .
C1 N1 C1 122.9(3) . 6
C1 N1 HN1 118.51(15) . .
C1 N1 HN1 118.51(15) 6 .
N1 C1 C2 119.9(2) . .
N1 C1 H1 120.1 . .
C2 C1 H1 120.1 . .
C2 C3 C2 120.5(3) . 6
C2 C3 Br1 119.71(13) . .
C2 C3 Br1 119.71(13) 6 .
C1 C2 C3 118.4(2) . .
C1 C2 H2 120.8 . .
C3 C2 H2 120.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Np1 O1 1.757(2) 5_667
Np1 O1 1.757(2) .
Np1 Cl1 2.6444(7) 5_667
Np1 Cl1 2.6444(7) .
Np1 Cl2 2.6517(7) 5_667
Np1 Cl2 2.6518(7) .
Br1 C3 1.872(3) .
N1 C1 1.340(2) .
N1 C1 1.340(2) 6
N1 HN1 0.879(18) .
C1 C2 1.371(3) .
C1 H1 0.9500 .
C3 C2 1.393(3) .
C3 C2 1.393(3) 6
C2 H2 0.9500 .
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
C1 N1 C1 C2 -0.7(4) 6
N1 C1 C2 C3 -0.8(3) .
C2 C3 C2 C1 2.3(4) 6
Br1 C3 C2 C1 -175.85(17) .
