Electroanalytical characterization of Np(VI)/Np(V) redox in a pentadentate ligand environment and stabilization of [Np<sup>V</sup>O<sub>2</sub>]<sup>+</sup> by hydrogen bonding.
Mikeska, Emily R.; Curry, T. Davis; Wilson, Richard E.; Blakemore, James D.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 19126–19142; doi:10.1039/d4dt02557a

data_7717312
_publ_section_title
;
 Electroanalytical characterization of Np(VI)/Np(V) redox in a
 pentadentate ligand environment and stabilization of
 [Np<sup>V</sup>O<sub>2</sub>]<sup>+</sup> by hydrogen bonding.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19126
_journal_page_last               19142
_journal_paper_doi               10.1039/d4dt02557a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         '2(C19 H21 N3 Np O4), 2(C16 H36 N), 3(H2 O)'
_chemical_formula_sum            'C70 H120 N8 Np2 O11'
_chemical_formula_weight         1723.73
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method
;FinalCif V139 by Daniel Kratzert, Freiburg 2024, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2024-07-31 deposited with the CCDC.	2024-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                93.5480(10)
_cell_angle_beta                 98.0660(10)
_cell_angle_gamma                94.4730(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9425(8)
_cell_length_b                   18.0802(15)
_cell_length_c                   21.1419(17)
_cell_measurement_reflns_used    6971
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.29
_cell_measurement_theta_min      2.3275
_cell_volume                     3741.2(5)
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ShelXle (H\"ubschle 2011)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 8.3
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 QUAZAR'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'glass fiber'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            45606
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.578
_diffrn_reflns_theta_min         0.975
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.6
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.822
_exptl_absorpt_correction_T_max  0.0932
_exptl_absorpt_correction_T_min  0.0641
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_description       prism
_exptl_crystal_F_000             1740
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_exptl_transmission_factor_max   0.0932
_exptl_transmission_factor_min   0.0641
_refine_diff_density_max         1.998
_refine_diff_density_min         -1.422
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     859
_refine_ls_number_reflns         15554
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0524
_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^)+(0.0539P)^2^+13.5120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1354
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11311
_reflns_number_total             15554
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02557a3.cif
_cod_data_source_block           m60a
_cod_depositor_comments
'Adding full bibliography for 7717312--7717314.cif.'
_cod_database_code               7717312
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.872
_shelx_estimated_absorpt_t_max   0.972
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 800'
_shelx_res_checksum              42889
_shelx_hkl_checksum              84279