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_4134695
_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 ad
_chemical_formula_moiety         'C60 H120 N16 P4 U1'
_chemical_formula_sum            'C60 H120 N16 P4 U'
_chemical_formula_weight         1427.62
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-06
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   20.6977(9)
_cell_length_b                   20.6977(9)
_cell_length_c                   14.1093(7)
_cell_measurement_reflns_used    9823
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.78
_cell_measurement_theta_min      2.69
_cell_volume                     5234.6(4)
_computing_data_collection       'APEX2 v2016.5-1 (Bruker, 2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.495
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16181
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.723
_diffrn_reflns_theta_min         3.103
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.465
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       prism
_exptl_crystal_F_000             2232
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.348
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.167
_refine_diff_density_max         1.802
_refine_diff_density_min         -1.389
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.53(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4925
_refine_ls_number_restraints     294
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1170P)^2^+4.0920P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1469
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                4887
_reflns_number_total             4925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c02693_si_002.cif
_cod_data_source_block           ntr-1-142
_cod_depositor_comments
'Adding full bibliography for 4134695--4134697.cif.'
_cod_original_cell_volume        5234.6(5)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4134695
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.47(3)
 0.53(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
3. Restrained distances
 C1_4-C3_4
 2.51 with sigma of 0.01
 N2_2-C1_2
 1.46 with sigma of 0.005
 C2_1-C1_1 = C3_1-C2_1 = C4_1-C3_1 = C4_1-C5_1 = C4_4-C5_4 = C3_4-C4_4 = C2_4-
 C3_4 = C2_4-C1_4 = C2_2-C1_2 = C2_2-C3_2 = C4_2-C3_2 = C4_2-C5_2
 1.525 with sigma of 0.005
 C1_3-C3_3
 2.51 with sigma of 0.01
 C5_3-C3_3
 2.52 with sigma of 0.01
 N2_4-C1_4 \\sim N2_4-C5_4
 N2_2-C1_2 \\sim N2_2-C5_2
 N2_1-C1_1 \\sim N2_1-C5_1
 N2_3-C1_3 \\sim N2_3-C5_3
 with sigma of 0.002
4. Uiso/Uaniso restraints and constraints
Uanis(C3_3) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C2_3) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(N1) \\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
 N2_4, C1_4, C2_4, C5_4, C3_4, C4_4
 N2_2, C1_2, C2_2, C5_2, C3_2, C4_2
 N2_1, C1_1, C2_1, C5_1, C3_1, C4_1
 N2_3, C1_3, C2_3, C5_3, C3_3, C4_3
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0002
 N2_2, C1_2, C2_2, C3_2, C4_2, C5_2
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0002
 P2, N2_2, N2_4
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0002
 N1, P2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N2_1, C1_1, C2_1, C3_1, C4_1, C5_1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N2_4
 N2_2
 N2_1
 N2_3
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0002
6. Same fragment restrains
{N2_2, C1_2, C2_2, C3_2, C4_2, C5_2}
{N2_1, C1_1, C2_1, C3_1, C4_1, C5_1}
{N2_3, C1_3, C2_3, C3_3, C4_3, C5_3}
as
{N2_4, C1_4, C2_4, C3_4, C4_4, C5_4} sigma for 1-2: 0.005 1-3: 0.01
7. Others
 Fixed U13: U1(0) N3(0) P1(0)
 Fixed U23: U1(0) N3(0) P1(0)
 Fixed X: U1(0) N3(0) P1(0)
 Fixed Y: U1(0) N3(0) P1(0)
8.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C1(H1A,H1B),
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C1(H1A,H1B), C2(H2A,H2B),
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B),
 C4(H4A,H4B), C5(H5A,H5B)
;
_shelx_res_checksum              65169
_shelx_hkl_checksum              64151
_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-1-142
_olex2_submission_special_instructions 'No special instructions were received'