Synthesis and Characterization of a Neutral U(II) Arene Sandwich Complex.
Billow, Brennan S.; Livesay, Brooke N.; Mokhtarzadeh, Charles C.; McCracken, John; Shores, Matthew P.; Boncella, James M.; Odom, Aaron L.; Journal of the American Chemical Society 140 (2018) 17369–17373; doi:10.1021/jacs.8b10888

data_4133539
_publ_section_title
;
 Synthesis and Characterization of a Neutral U(II) Arene Sandwich Complex.
;
_journal_issue                   50
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17369
_journal_page_last               17373
_journal_paper_doi               10.1021/jacs.8b10888
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C72 H100 I N2 U, 0.5(C4 H10 O)'
_chemical_formula_sum            'C74 H105 I N2 O0.5 U'
_chemical_formula_weight         1395.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.0070(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2986(7)
_cell_length_b                   23.8567(11)
_cell_length_c                   18.6523(9)
_cell_measurement_reflns_used    9957
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.74
_cell_measurement_theta_min      2.36
_cell_volume                     6770.2(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0388
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            82390
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.356
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.895
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.0569 before and 0.0442 after correction. The Ratio of minimum to maximum transmission is 0.8674. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       Block
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         16801
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+4.4987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0552
_refine_ls_wR_factor_ref         0.0593
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13702
_reflns_number_total             16801
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b10888_si_002.cif
_cod_data_source_block           trippnh2ui
_cod_original_formula_sum        'C74 H105 I N2 O0.50 U'
_cod_database_code               4133539
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.671
_shelx_estimated_absorpt_t_min   0.624
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C1A-C1B \\sim C1C-C1D
 with sigma of 0.02
 O2-C1B \\sim O2-C1C
 with sigma of 0.02
 C1A-O2 \\sim O2-C1D
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O2 \\sim C1A \\sim C1B \\sim C1C \\sim C1D: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 O2, C1A, C1B, C1C, C1D
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C61, C67, C67A, C69, C69A, C68
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H68A(0.5) H68B(0.5) H68C(0.5) H68D(0.5) H68E(0.5) H68F(0.5)
 C67A(0.5) H67A(0.5) C70A(0.5) H70A(0.5) C71A(0.5) H71A(0.5) H71B(0.5)
 H71C(0.5) C72A(0.5) H72A(0.5) H72B(0.5) H72C(0.5) C69A(0.5) H69A(0.5)
 H69B(0.5) H69C(0.5) C71(0.5) H71D(0.5) H71E(0.5) H71F(0.5) C70(0.5) H70(0.5)
 C72(0.5) H72D(0.5) H72E(0.5) H72F(0.5) C69(0.5) H69D(0.5) H69E(0.5) H69F(0.5)
 C67(0.5) H67(0.5) O2(0.5) C1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C1B(0.5)
 H1BA(0.5) H1BB(0.5) C1C(0.5) H1CA(0.5) H1CB(0.5) C1D(0.5) H1DA(0.5) H1DB(0.5)
 H1DC(0.5)
6.a Ternary CH refined with riding coordinates:
 C13(H13), C49(H49), C55(H55), C53(H53), C19(H19), C16(H16), C28(H28),
 C31(H31), C34(H34), C64(H64), C67A(H67A), C70A(H70A), C70(H70), C67(H67)
6.b Secondary CH2 refined with riding coordinates:
 C1B(H1BA,H1BB), C1C(H1CA,H1CB)
6.c Me refined with riding coordinates:
 C68(H68A,H68B,H68C), C68(H68D,H68E,H68F)
6.d Aromatic/amide H refined with riding coordinates:
 C45(H45), C47(H47), C39(H39), C40(H40), C41(H41), C9(H9), C11(H11), C3(H3),
 C4(H4), C5(H5), C24(H24), C26(H26), C60(H60), C62(H62)
6.e Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C51(H51A,H51B,H51C), C50(H50A,H50B,H50C), C57(H57A,H57B,
 H57C), C56(H56A,H56B,H56C), C54(H54A,H54B,H54C), C52(H52A,H52B,H52C), C14(H14A,
 H14B,H14C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C17(H17A,H17B,H17C),
 C18(H18A,H18B,H18C), C30(H30A,H30B,H30C), C29(H29A,H29B,H29C), C33(H33A,H33B,
 H33C), C32(H32A,H32B,H32C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C66(H66A,
 H66B,H66C), C65(H65A,H65B,H65C), C71A(H71A,H71B,H71C), C72A(H72A,H72B,H72C),
 C69A(H69A,H69B,H69C), C71(H71D,H71E,H71F), C72(H72D,H72E,H72F), C69(H69D,H69E,
 H69F), C1A(H1AA,H1AB,H1AC), C1D(H1DA,H1DB,H1DC)
;
_shelx_res_checksum              76206
_shelx_hkl_checksum              89905
_olex2_submission_special_instructions 'No special instructions were received'