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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/4/12/63/4126311.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_4126311
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 Cl 1+)2, (Np O2 Cl4 2-)'
_chemical_formula_sum            'C10 H10 Cl6 N2 Np O2'
_chemical_formula_weight         639.90
_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                 105.585(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.7687(10)
_cell_length_b                   6.7068(4)
_cell_length_c                   9.0971(6)
_cell_measurement_reflns_used    3441
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      52.235
_cell_measurement_theta_min      6.082
_cell_volume                     926.71(10)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture'
_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  0.0382
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7582
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.731
_diffrn_reflns_theta_min         3.041
_diffrn_source                   'Fine-Focus Sealed Tube'
_exptl_absorpt_coefficient_mu    6.473
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Krause et. al 2015'
_exptl_crystal_colour            Yellow-Green
_exptl_crystal_density_diffrn    2.293
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             590
_exptl_crystal_recrystallization_method 'Acidic (HCl) aqueous evaporation'
_exptl_crystal_size_max          0.229
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.032
_refine_diff_density_max         0.817
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     64
_refine_ls_number_reflns         1307
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0248
_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)+(0.0191P)²+0.9044P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0457
_refine_ls_wR_factor_ref         0.0462
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1281
_reflns_number_total             1307
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja7b05689_si_002.cif
_cod_data_source_block           Compound_6
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4126311
_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   0.319
_shelx_estimated_absorpt_t_max   0.820
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 0.1888(3) 0.0000 0.6106(6) 0.0572(13) Uani 1 2 d S T P
H1 H 0.1275 0.0000 0.5811 0.069 Uiso 1 2 calc R U P
C2 C 0.2342(3) 0.0000 0.5038(5) 0.0500(11) Uani 1 2 d S T P
H2 H 0.2051 0.0000 0.4003 0.060 Uiso 1 2 calc R U P
C3 C 0.3248(3) 0.0000 0.5528(6) 0.0494(11) Uani 1 2 d S T P
C4 C 0.3685(3) 0.0000 0.7050(6) 0.0618(14) Uani 1 2 d S T P
H4 H 0.4297 0.0000 0.7373 0.074 Uiso 1 2 calc R U P
C5 C 0.3193(4) 0.0000 0.8080(6) 0.0665(15) Uani 1 2 d S T P
H5 H 0.3467 0.0000 0.9121 0.080 Uiso 1 2 calc R U P
N1 N 0.2321(3) 0.0000 0.7581(5) 0.0590(11) Uani 1 2 d S T P
HN1 H 0.2020 0.0000 0.8243 0.071 Uiso 1 2 calc R U P
O1 O 0.0000 -0.2593(6) 0.0000 0.0696(10) Uani 1 2 d S T P
Cl1 Cl 0.17631(7) 0.0000 0.06980(13) 0.0577(3) Uani 1 2 d S T P
Cl2 Cl 0.00737(9) 0.0000 0.29175(15) 0.0917(6) Uani 1 2 d S T P
Cl3 Cl 0.38354(10) 0.0000 0.4192(2) 0.0822(5) Uani 1 2 d S T P
Np1 Np 0.0000 0.0000 0.0000 0.03936(9) 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 0.0033 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'
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(5) . .
N1 C1 H1 120.1 . .
C2 C1 H1 120.1 . .
C1 C2 C3 118.1(4) . .
C1 C2 H2 120.9 . .
C3 C2 H2 120.9 . .
C4 C3 C2 121.5(5) . .
C4 C3 Cl3 119.7(4) . .
C2 C3 Cl3 118.8(4) . .
C5 C4 C3 117.9(5) . .
C5 C4 H4 121.0 . .
C3 C4 H4 121.0 . .
N1 C5 C4 119.5(5) . .
N1 C5 H5 120.3 . .
C4 C5 H5 120.3 . .
C5 N1 C1 123.2(5) . .
C5 N1 HN1 118.4 . .
C1 N1 HN1 118.4 . .
O1 Np1 O1 180.0 5 .
O1 Np1 Cl2 90.0 5 5
O1 Np1 Cl2 90.0 . 5
O1 Np1 Cl2 90.0 5 .
O1 Np1 Cl2 90.0 . .
Cl2 Np1 Cl2 180.0 5 .
O1 Np1 Cl1 90.0 5 .
O1 Np1 Cl1 90.0 . .
Cl2 Np1 Cl1 90.05(4) 5 .
Cl2 Np1 Cl1 89.95(4) . .
O1 Np1 Cl1 90.0 5 5
O1 Np1 Cl1 90.0 . 5
Cl2 Np1 Cl1 89.95(4) 5 5
Cl2 Np1 Cl1 90.05(4) . 5
Cl1 Np1 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
C1 N1 1.333(7) .
C1 C2 1.352(7) .
C1 H1 0.9300 .
C2 C3 1.378(6) .
C2 H2 0.9300 .
C3 C4 1.371(7) .
C3 Cl3 1.714(5) .
C4 C5 1.368(8) .
C4 H4 0.9300 .
C5 N1 1.327(7) .
C5 H5 0.9300 .
N1 HN1 0.8600 .
O1 Np1 1.739(4) .
Cl1 Np1 2.6803(11) .
Cl2 Np1 2.6253(14) .
Np1 O1 1.739(4) 5
Np1 Cl2 2.6252(14) 5
Np1 Cl1 2.6804(11) 5
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 Cl2 0.93 2.80 3.484(5) 131.2 .
C1 H1 Cl2 0.93 2.68 3.440(5) 139.3 5_556
C2 H2 Cl1 0.93 2.92 3.806(5) 160.2 .
N1 HN1 Cl1 0.86 2.37 3.186(5) 157.4 1_556
C1 H1 Cl2 0.93 2.80 3.484(5) 131.2 .
C1 H1 Cl2 0.93 2.68 3.440(5) 139.3 5_556
C2 H2 Cl1 0.93 2.92 3.806(5) 160.2 .
N1 HN1 Cl1 0.86 2.37 3.186(5) 157.4 1_556
