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_7122282
_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         'C126 H180 O12 Se4 U2, C6'
_chemical_formula_sum            'C154 H212 O12 Se4 U2'
_chemical_formula_weight         3047.12
_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
_audit_creation_date             2018-08-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-01 deposited with the CCDC.
2018-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                102.6420(10)
_cell_angle_beta                 98.5580(10)
_cell_angle_gamma                114.9460(10)
_cell_formula_units_Z            1
_cell_length_a                   14.3383(9)
_cell_length_b                   14.4734(9)
_cell_length_c                   21.5834(19)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.20
_cell_measurement_theta_min      2.16
_cell_volume                     3812.7(5)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            41560
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.389
_diffrn_reflns_theta_min         1.628
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.130
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5153
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1021 before and 0.0422 after correction. The Ratio of minimum to maximum transmission is 0.6913. The \l/2 correction factor is 0.0015.'
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_description       plate
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.675
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     717
_refine_ls_number_reflns         15513
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0482P)^2^+3.2416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.0968
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12923
_reflns_number_total             15513
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc05244a2.cif
_cod_data_source_block           mel_sq
_cod_depositor_comments
'Adding full bibliography for 7122280--7122282.cif.'
_cod_database_code               7122282
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.859
_shelx_estimated_absorpt_t_min   0.508
_olex2_refinement_description
;
1. 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
2. Others
 Sof(C36B)=Sof(H36D)=Sof(H36E)=Sof(H36F)=Sof(C38B)=Sof(H38D)=Sof(H38E)=
 Sof(H38F)=Sof(C37B)=Sof(H37D)=Sof(H37E)=Sof(H37F)=1-FVAR(1)
 Sof(C37A)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C38A)=Sof(H38A)=Sof(H38B)=
 Sof(H38C)=Sof(C36A)=Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(1)
 Sof(C42B)=Sof(H42D)=Sof(H42E)=Sof(H42F)=Sof(C41B)=Sof(H41D)=Sof(H41E)=
 Sof(H41F)=Sof(C40B)=Sof(H40D)=Sof(H40E)=Sof(H40F)=1-FVAR(2)
 Sof(C40A)=Sof(H40A)=Sof(H40B)=Sof(H40C)=Sof(C42A)=Sof(H42A)=Sof(H42B)=
 Sof(H42C)=Sof(C41A)=Sof(H41A)=Sof(H41B)=Sof(H41C)=FVAR(2)
 Fixed Sof: C3S(0.5) C1S(0.5) C6S(0.5) C2S(0.5) C5S(0.5) C4S(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C60(H60A,H60B), C63(H63A,H63B), C61(H61A,H61B), C62(H62A,H62B)
3.b Me refined with riding coordinates:
 C37A(H37A,H37B,H37C), C40A(H40A,H40B,H40C), C42A(H42A,H42B,H42C), C38A(H38A,
 H38B,H38C), C36A(H36A,H36B,H36C), C41A(H41A,H41B,H41C), C42B(H42D,H42E,H42F),
 C36B(H36D,H36E,H36F), C41B(H41D,H41E,H41F), C38B(H38D,H38E,H38F), C37B(H37D,
 H37E,H37F), C40B(H40D,H40E,H40F)
3.c Aromatic/amide H refined with riding coordinates:
 C45(H45), C47(H47), C31(H31), C59(H59), C33(H33), C58(H58), C19(H19), C3(H3),
 C5(H5), C17(H17)
3.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C55(H55A,H55B,H55C), C83(H83A,H83B,
 H83C), C14(H14A,H14B,H14C), C56(H56A,H56B,H56C), C12(H12A,H12B,H12C), C13(H13A,
 H13B,H13C), C28(H28A,H28B,H28C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C),
 C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C8A(H8AA,H8AB,
 H8AC), C10A(H10A,H10B,H10C), C9A(H9AA,H9AB,H9AC), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              48373
_shelx_fab_checksum              42807
_olex2_submission_special_instructions 'No special instructions were received'