Complexation and redox chemistry of neptunium, plutonium and americium with a hydroxylaminato ligand
Su, Jing; Cheisson, Thibault; McSkimming, Alex; Goodwin, Conrad A. P.; DiMucci, Ida M.; Albrecht-Schönzart, Thomas; Scott, Brian L.; Batista, Enrique R.; Gaunt, Andrew J.; Kozimor, Stosh A.; Yang, Ping; Schelter, Eric J.; Chemical Science  (2021) –; doi:10.1039/D1SC03905A

data_1564665
_publ_section_title
;
 Complexation and redox chemistry of neptunium, plutonium and americium
 with a hydroxylaminato ligand
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC03905A
_journal_year                    2021
_chemical_formula_moiety         'C54 H78 Am2 N12 O6'
_chemical_formula_sum            'C54 H78 Am2 N12 O6'
_chemical_formula_weight         1477.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-01-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-01-15 deposited with the CCDC.	2021-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.1463(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.9096(17)
_cell_length_b                   16.627(2)
_cell_length_c                   13.5557(18)
_cell_measurement_reflns_used    7145
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      24.89
_cell_measurement_theta_min      2.42
_cell_volume                     2854.8(6)
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_collection       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS 2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            28632
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.778
_diffrn_reflns_theta_min         1.961
_exptl_absorpt_coefficient_mu    2.725
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v. 2.03 (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_description       plate
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.646
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         5455
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+1.4914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0611
_refine_ls_wR_factor_ref         0.0668
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4241
_reflns_number_total             5455
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc03905a2.cif
_cod_data_source_block           3
_cod_original_cell_volume        2854.8(7)
_cod_database_code               1564665
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.772
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C6-C7 = C6-C8 = C6-C9 = C6-C7' = C6-C8' = C6-C9'
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C7') \\sim
Ueq, Uanis(C8') \\sim Ueq, Uanis(C9') \\sim Ueq: with sigma of 0.005 and sigma
for terminal atoms of 0.007
4. Others
 Fixed Sof: C7(0.5) H7A(0.5) H7B(0.5) H7C(0.5) C8(0.5) H8A(0.5) H8B(0.5)
 H8C(0.5) C9(0.5) H9A(0.5) H9B(0.5) H9C(0.5) C7'(0.5) H7'A(0.5) H7'B(0.5)
 H7'C(0.5) C8'(0.5) H8'A(0.5) H8'B(0.5) H8'C(0.5) C9'(0.5) H9'A(0.5) H9'B(0.5)
 H9'C(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C10(H10), C11(H11), C12(H12), C13(H13),
 C19(H19), C20(H20), C21(H21), C22(H22)
5.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C7'(H7'A,H7'B,H7'C),
 C8'(H8'A,H8'B,H8'C), C9'(H9'A,H9'B,H9'C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C)
;
_shelx_res_checksum              27260
_shelx_hkl_checksum              2438
_olex2_submission_special_instructions 'No special instructions were received'