Transuranic Hybrid Materials: Crystallographic and Computational Metrics of Supramolecular Assembly.
Surbella, Robert G.; Ducati, Lucas Colucci; Pellegrini, Kristi L.; McNamara, Bruce K.; Autschbach, Jochen; Schwantes, Jon Michael; Cahill, Christopher L.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b05689

data_4126312
_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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.0127P)^2^+1.3918P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_res_checksum              34921
_shelx_hkl_checksum              41414