Two-Electron Oxidative Atom Transfer at a Homoleptic, Tetravalent Uranium Complex.
Rice, Natalie T.; McCabe, Karl; Bacsa, John; Maron, Laurent; La Pierre, Henry S.; Journal of the American Chemical Society 142 (2020) 7368–7373; doi:10.1021/jacs.0c02693

data_4134696
_publ_section_title
;
 Two-Electron Oxidative Atom Transfer at a Homoleptic, Tetravalent Uranium
 Complex.
;
_journal_issue                   16
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7368
_journal_page_last               7373
_journal_paper_doi               10.1021/jacs.0c02693
_journal_volume                  142
_journal_year                    2020
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C60 H120 N16 O1 P4 U1'
_chemical_formula_sum            'C60 H120 N16 O P4 U'
_chemical_formula_weight         1443.62
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-01-20
_audit_creation_method
;
Olex2 1.3-alpha
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   20.770(3)
_cell_length_b                   20.770(3)
_cell_length_c                   13.975(2)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    103.58
_cell_measurement_theta_max      21.79
_cell_measurement_theta_min      2.69
_cell_volume                     5221.0(13)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      103.58
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_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  0.0476
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27505
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.480
_diffrn_reflns_theta_min         2.693
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.474
_exptl_absorpt_correction_T_max  0.5644
_exptl_absorpt_correction_T_min  0.4780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0914 before and 0.0823 after correction.
The Ratio of minimum to maximum transmission is 0.8469.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       prism
_exptl_crystal_F_000             2256
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.333
_exptl_crystal_size_mid          0.276
_exptl_crystal_size_min          0.262
_refine_diff_density_max         1.364
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.239
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_coef       0.0046(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         6437
_refine_ls_number_restraints     413
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0605
_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^)+(0.1182P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1498
_refine_ls_wR_factor_ref         0.1561
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                5935
_reflns_number_total             6437
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c02693_si_004.cif
_cod_data_source_block           ntr-4-081
_cod_depositor_comments
'Adding full bibliography for 4134695--4134697.cif.'
_cod_original_cell_volume        5220.9(16)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4134696
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.59(3)
 -0.032(15) 0.43(2) 0.008(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
3. Restrained distances
 P1-N1_1 = P1-N1_3 = P1-N1_2
 1.691 with sigma of 0.005
 P2-N3
 1.53 with sigma of 0.003
 C5_4-C4_4 \\sim C4_4-C3_4 \\sim C3_4-C2_4 \\sim C6_4-C5_4 \\sim C3_1-C2_1
\\sim C6_1-C5_1 \\sim C3_2-
 C2_2 \\sim C6_2-C5_2 \\sim C3_3-C2_3 \\sim C6_3-C5_3 \\sim C4_1-C3_1 \\sim
C5_1-C4_1 \\sim C4_2-C3_2 ~
 C5_2-C4_2 \\sim C4_3-C3_3 \\sim C5_3-C4_3
 with sigma of 0.002
 N1_4-C2_4 \\sim N1_4-C6_4 \\sim N1_1-C2_1 \\sim N1_1-C6_1 \\sim N1_2-C2_2
\\sim N1_2-C6_2 \\sim N1_3-
 C2_3 \\sim N1_3-C6_3
 with sigma of 0.002
4. Uiso/Uaniso restraints and constraints
Uanis(N2) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(N3) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
5. Rigid body (RIGU) restrains
 N1_1, C2_1, C3_1, C4_1, C5_1, C6_1
 N1_2, C2_2, C3_2, C4_2, C5_2, C6_2
 N1_3, C2_3, C3_3, C4_3, C5_3, C6_3
 N1_4, C2_4, C3_4, C4_4, C5_4, C6_4
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0004
 U1, N3
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0004
 P2, N3
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0002
 P1, N3, U1, P2, O1, N2, N1_4, C2_4, C6_4, N1_1, N1_2, N1_3, C3_4, C5_4, C2_1,
 C6_1, C2_2, C6_2, C2_3, C6_3, C4_4, C3_1, C5_1, C3_2, C5_2, C3_3, C5_3, C4_1,
 C4_2, C4_3
 with sigma for 1-2 distances of 0.0004 and sigma for 1-3 distances of 0.0004
6. Same fragment restrains
{N1_2, C2_2, C3_2, C4_2, C5_2, C6_2}
{N1_3, C2_3, C3_3, C4_3, C5_3, C6_3}
{N1_4, C2_4, C3_4, C4_4, C5_4, C6_4}
as
{N1_1, C2_1, C3_1, C4_1, C5_1, C6_1} sigma for 1-2: 0.002 1-3: 0.002
7.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C2(H2A,H2B),
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C2(H2A,H2B), C3(H3A,H3B),
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B),
 C5(H5A,H5B), C6(H6A,H6B)
;
_shelx_res_checksum              40039
_shelx_hkl_checksum              30644
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id NTR-4-081
_olex2_submission_special_instructions 'No special instructions were received'