Two-electron oxidation of a homoleptic U(iii) guanidinate complex by diphenyldiazomethane.
Settineri, Nicholas S.; Shiau, Angela A.; Arnold, John; Chemical communications (Cambridge, England) 54 (2018) 10913–10916; doi:10.1039/c8cc06514d

data_7122335
_publ_section_title
;
 Two-electron oxidation of a homoleptic U(iii) guanidinate complex by
 diphenyldiazomethane.
;
_journal_issue                   77
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10913
_journal_page_last               10916
_journal_paper_doi               10.1039/c8cc06514d
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C39 H84 N12 U'
_chemical_formula_sum            'C39 H84 N12 U'
_chemical_formula_weight         959.21
_chemical_name_common            U(N3)(TIG)3
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-08-07 deposited with the CCDC.
2018-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                96.1010(10)
_cell_angle_beta                 103.8660(10)
_cell_angle_gamma                119.6380(10)
_cell_formula_units_Z            2
_cell_length_a                   13.0981(2)
_cell_length_b                   13.2024(2)
_cell_length_c                   17.7597(2)
_cell_measurement_reflns_used    34744
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.8460
_cell_measurement_theta_min      3.4830
_cell_volume                     2497.88(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45f (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45f (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45f (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.861
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            58226
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.861
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.678
_diffrn_reflns_theta_min         3.140
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    3.286
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35101
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Olex2 1.2-ac3
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       block
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.798
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         12188
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0232
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0224P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0515
_refine_ls_wR_factor_ref         0.0522
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11244
_reflns_number_total             12188
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc06514d2.cif
_cod_data_source_block           U(N3)(TIG)3
_cod_depositor_comments
'Adding full bibliography for 7122334--7122339.cif.'
_cod_database_code               7122335
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.589
_shelx_estimated_absorpt_t_max   0.639
_shelx_res_checksum              9590
_shelx_fab_checksum              89481