Structure and properties of [(4,6-<sup>t</sup>Bu<sub>2</sub>C<sub>6</sub>H<sub>2</sub>O)<sub>2</sub>Se]<sub>2</sub>An(THF)<sub>2</sub>, An = U, Np, and their reaction with p-benzoquinone.
Myers, Alexander J.; Rungthanaphatsophon, Pokpong; Behrle, Andrew C.; Vilanova, Sean P.; Kelley, Stephen P.; Lukens, Wayne W.; Walensky, Justin R.; Chemical communications (Cambridge, England) 54 (2018) 10435–10438; doi:10.1039/c8cc05244a

data_7122281
_publ_section_title
;
 Structure and properties of
 [(4,6-<sup>t</sup>Bu<sub>2</sub>C<sub>6</sub>H<sub>2</sub>O)<sub>2</sub>Se]<sub>2</sub>An(THF)<sub>2</sub>,
 An = U, Np, and their reaction with p-benzoquinone.
;
_journal_issue                   74
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10435
_journal_page_last               10438
_journal_paper_doi               10.1039/c8cc05244a
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C64 H96 Np O6 Se2, 2(C7 H8)'
_chemical_formula_sum            'C78 H112 Np O6 Se2'
_chemical_formula_weight         1540.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-06-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-26 deposited with the CCDC.
2018-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.9910(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5780(12)
_cell_length_b                   20.5093(15)
_cell_length_c                   21.1111(15)
_cell_measurement_reflns_used    9761
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.42
_cell_measurement_theta_min      2.23
_cell_volume                     7351.8(9)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_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  0.0907
_diffrn_reflns_av_unetI/netI     0.0938
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            121346
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.418
_diffrn_reflns_theta_min         0.998
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.453
_exptl_absorpt_correction_T_max  0.5624
_exptl_absorpt_correction_T_min  0.4773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       plate
_exptl_crystal_F_000             3156
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.076
_refine_diff_density_max         4.403
_refine_diff_density_min         -3.078
_refine_diff_density_rms         0.194
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.473(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1422
_refine_ls_number_reflns         29482
_refine_ls_number_restraints     1636
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.1101
_refine_ls_R_factor_gt           0.0722
_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^)+(0.0173P)^2^+43.2237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1193
_reflns_Friedel_coverage         0.943
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                21344
_reflns_number_total             29482
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc05244a2.cif
_cod_data_source_block           s2_b
_cod_depositor_comments
'Adding full bibliography for 7122280--7122282.cif.'
_cod_database_code               7122281
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.836
_shelx_estimated_absorpt_t_min   0.379
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.527(16)
 0.473(16)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(O6A) = Uanis(O5B)
Uanis(O5B) = Uanis(O6A)
Uanis(O3B) = Uanis(O3A)
Uanis(O4B) = Uanis(O4A)
Uanis(C67B) = Uanis(C60A)
Uanis(C57A) = Uanis(C60B)
Uanis(C58A) = Uanis(C59B)
Uanis(C59A) = Uanis(C58B)
Uanis(C29B) = Uanis(C29A)
Uanis(C34B) = Uanis(C30A)
Uanis(C33B) = Uanis(C31A)
Uanis(C32B) = Uanis(C32A)
Uanis(C33A) = Uanis(C31B)
Uanis(C30B) = Uanis(C34A)
Uanis(C43A) = Uanis(C43B)
Uanis(C48A) = Uanis(C48B)
Uanis(C47A) = Uanis(C47B)
Uanis(C46B) = Uanis(C46A)
Uanis(C45B) = Uanis(C45A)
Uanis(C44B) = Uanis(C44A)
Uanis(O5A) = Uanis(O6B)
Uanis(O1B) = Uanis(O2A)
Uanis(O1A) = Uanis(O2B)
Uanis(C61B) = Uanis(C61A)
Uanis(C62A) = Uanis(C62B)
Uanis(C63B) = Uanis(C63A)
Uanis(C64B) = Uanis(C64A)
Uanis(C1B) = Uanis(C15A)
Uanis(C20A) = Uanis(C6B)
Uanis(C2B) = Uanis(C16A)
Uanis(C17A) = Uanis(C3B)
Uanis(C4B) = Uanis(C18A)
Uanis(C19A) = Uanis(C5B)
Uanis(C1A) = Uanis(C15B)
Uanis(C2A) = Uanis(C16B)
Uanis(C3A) = Uanis(C17B)
Uanis(C18B) = Uanis(C4A)
Uanis(C19B) = Uanis(C5A)
Uanis(C20B) = Uanis(C6A)
Uanis(C15B) = Uanis(C1A)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C42B(0.5) H42A(0.5) H42B(0.5) H42C(0.5) C41B(0.5) H41A(0.5)
 H41B(0.5) H41C(0.5) C40B(0.5) H40A(0.5) H40B(0.5) H40C(0.5) C40'(0.5)
 H40D(0.5) H40E(0.5) H40F(0.5) C42'(0.5) H42D(0.5) H42E(0.5) H42F(0.5)
 C41'(0.5) H41D(0.5) H41E(0.5) H41F(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C57A(H57C,H57D), C64A(H64C,H64D), C63A(H63C,H63D), C57B(H57A,H57B), C64B(H64A,
 H64B), C61A(H61C,H61D), C63B(H63A,H63B), C60B(H60A,H60B), C60A(H60C,H60D),
 C61B(H61A,H61B), C58A(H58C,H58D), C59B(H59A,H59B), C59A(H59C,H59D), C58B(H58A,
 H58B), C62B(H62A,H62B), C62A(H62C,H62D)
6.b Aromatic/amide H refined with riding coordinates:
 C17A(H17A), C31A(H31A), C33B(H33B), C31B(H31B), C3B(H3B), C5A(H5A),
 C19A(H19A), C45B(H45B), C47A(H47A), C45A(H45A), C74B(H74B), C3A(H3A),
 C76B(H76B), C5B(H5B), C73A(H73A), C47B(H47B), C19B(H19B), C17B(H17B),
 C77B(H77B), C77A(H77A), C33A(H33A), C70B(H70B), C66A(H66A), C73B(H73B),
 C74A(H74A), C75A(H75A), C66B(H66B), C75B(H75B), C67A(H67A), C76A(H76A),
 C68A(H68A), C69B(H69B), C70A(H70A), C68B(H68B), C69A(H69A), C67B(H67B)
6.c Idealised Me refined as rotating group:
 C14A(H14D,H14E,H14F), C22A(H22D,H22E,H22F), C54A(H54D,H54E,H54F), C36A(H36D,
 H36E,H36F), C9A(H9AA,H9AB,H9AC), C9B(H9BA,H9BB,H9BC), C13A(H13D,H13E,H13F),
 C54B(H54A,H54B,H54C), C37A(H37D,H37E,H37F), C27A(H27D,H27E,H27F), C51A(H51D,
 H51E,H51F), C26A(H26D,H26E,H26F), C28B(H28A,H28B,H28C), C24A(H24D,H24E,H24F),
 C12B(H12A,H12B,H12C), C56B(H56A,H56B,H56C), C52B(H52A,H52B,H52C), C24B(H24A,
 H24B,H24C), C26B(H26A,H26B,H26C), C10B(H10A,H10B,H10C), C55A(H55D,H55E,H55F),
 C38A(H38D,H38E,H38F), C23A(H23D,H23E,H23F), C13B(H13A,H13B,H13C), C78A(H78D,
 H78E,H78F), C12A(H12D,H12E,H12F), C8B(H8BA,H8BB,H8BC), C56A(H56D,H56E,H56F),
 C52A(H52D,H52E,H52F), C50A(H50D,H50E,H50F), C51B(H51A,H51B,H51C), C71B(H71D,
 H71E,H71F), C28A(H28D,H28E,H28F), C42A(H42G,H42H,H42I), C55B(H55A,H55B,H55C),
 C78B(H78A,H78B,H78C), C38B(H38A,H38B,H38C), C23B(H23A,H23B,H23C), C22B(H22A,
 H22B,H22C), C8A(H8AA,H8AB,H8AC), C27B(H27A,H27B,H27C), C14B(H14A,H14B,H14C),
 C37B(H37A,H37B,H37C), C50B(H50A,H50B,H50C), C10A(H10D,H10E,H10F), C36B(H36A,
 H36B,H36C), C40A(H40G,H40H,H40I), C41A(H41G,H41H,H41I), C42B(H42A,H42B,H42C),
 C41B(H41A,H41B,H41C), C40B(H40A,H40B,H40C), C71A(H71A,H71B,H71C), C40'(H40D,
 H40E,H40F), C42'(H42D,H42E,H42F), C41'(H41D,H41E,H41F)
;
_shelx_res_checksum              73490
_olex2_submission_special_instructions 'No special instructions were received'