Structures of Plutonium(IV) and Uranium(VI) with N,N-Dialkyl Amides from Crystallography, X-ray Absorption Spectra, and Theoretical Calculations.
Acher, Eléonor; Hacene Cherkaski, Yanis; Dumas, Thomas; Tamain, Christelle; Guillaumont, Dominique; Boubals, Nathalie; Javierre, Guilhem; Hennig, Christoph; Solari, Pier Lorenzo; Charbonnel, Marie-Christine; Inorganic chemistry 55 (2016) 5558–5569; doi:10.1021/acs.inorgchem.6b00592

data_4347777
_publ_section_title
;
 Structures of Plutonium(IV) and Uranium(VI) with N,N-Dialkyl Amides from
 Crystallography, X-ray Absorption Spectra, and Theoretical Calculations.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5558
_journal_page_last               5569
_journal_paper_doi               10.1021/acs.inorgchem.6b00592
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C24 Ce N6 O14'
_chemical_formula_weight         736.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 110.5780(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.3316(15)
_cell_length_b                   10.8597(5)
_cell_length_c                   20.3225(9)
_cell_measurement_reflns_used    4962
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.11
_cell_measurement_theta_min      2.35
_cell_volume                     7300.0(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-13 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-13 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35313
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.532
_diffrn_reflns_theta_max         24.532
_diffrn_reflns_theta_min         1.974
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    1.309
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_exptl_transmission_factor_max   0.7451
_exptl_transmission_factor_min   0.6079
_refine_diff_density_max         1.114
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6087
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0612
_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/[\s^2^(Fo^2^)+(0.1122P)^2^+20.0303P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1651
_refine_ls_wR_factor_ref         0.1937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4111
_reflns_number_total             6087
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00592_si_003.cif
_cod_data_source_block           YHC-CT-DBBA-Ce-10
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4347777
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.828
_shelx_estimated_absorpt_t_max   0.974
_shelx_res_checksum              37510
_shelx_hkl_checksum              78393