Unveiling the covalency of versatile Pu(iii)-N bonds in a unique plutonium(iii) complex
Bai, Zhuanling; Martelles, Madeline C.; Sperling, Joseph M.; Albrecht, Thomas E.; Chemical Science 16 (2025) 10424–10431; doi:10.1039/D5SC01808K

data_1574580
_publ_section_title
;
 Unveiling the covalency of versatile Pu(iii)-N bonds in a unique
 plutonium(iii) complex
;
_journal_issue                   23
_journal_name_full               'Chemical Science'
_journal_page_first              10424
_journal_page_last               10431
_journal_paper_doi               10.1039/D5SC01808K
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C18 H29 N30 Na2 O12 Pu, H2 O'
_chemical_formula_sum            'C18 H31 N30 Na2 O13 Pu'
_chemical_formula_weight         1163.71
_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     iterative
_audit_creation_date             2025-02-17
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-02-18 deposited with the CCDC.	2025-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                88.144(2)
_cell_angle_beta                 74.108(2)
_cell_angle_gamma                79.653(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5590(5)
_cell_length_b                   14.5429(8)
_cell_length_c                   14.7750(8)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.44
_cell_volume                     1943.02(18)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0522
_diffrn_reflns_av_unetI/netI     0.0646
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23016
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.002
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.819
_exptl_absorpt_correction_T_max  0.6468
_exptl_absorpt_correction_T_min  0.4915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1035 before and 0.0528 after correction.
The Ratio of minimum to maximum transmission is 0.7599.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.989
_exptl_crystal_description       needle
_exptl_crystal_F_000             1138
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.034
_exptl_crystal_size_min          0.01
_refine_diff_density_max         4.013
_refine_diff_density_min         -4.797
_refine_diff_density_rms         0.235
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         8912
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0176P)^2^+27.6657P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1172
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8065
_reflns_number_total             8912
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01808k2.cif
_cod_data_source_block           pu_dtp
_cod_depositor_comments          'Adding full bibliography for 1574580.cif.'
_cod_database_code               1574580
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.772
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9878(5)
 0.0122(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 H5B-H30
 2.12 with sigma of 0.01
 H11A_$6-H8B
 2.12 with sigma of 0.01
 H8A-H11A_$6
 2.12 with sigma of 0.01
 Pu1-H1A \\sim Pu1-H1B
 with sigma of 0.02
 Na1-H12A \\sim Na1-H12B
 with sigma of 0.02
4. Others
 Fixed Sof: Na2(0.5) Na7(0.5)
5.a Free rotating group:
 O1(H1A,H1B), O5(H5A,H5B), O12(H12A,H12B)
5.b Rotating group:
 O2(H2A,H2B), O3(H3A,H3B), O4(H4A,H4B), O11(H11A,H11B), O6(H6A,H6B), O10(H10A,
 H10B), O9(H9A,H9B), O8(H8A,H8B), O13(H13A,H13B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), N30(H30), C4(H4), C10(H10), C9(H9), C16(H16), C15(H15)
;
_shelx_res_checksum              33614
_olex2_submission_special_instructions 'No special instructions were received'