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_4133540
_publ_section_title
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 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 N2 U, C4 H8 O'
_chemical_formula_sum            'C76 H108 N2 O U'
_chemical_formula_weight         1303.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                 106.9720(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0536(13)
_cell_length_b                   16.8949(12)
_cell_length_c                   22.7572(16)
_cell_measurement_reflns_used    9854
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.218
_cell_measurement_theta_min      2.411
_cell_volume                     6639.0(8)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0396
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            39160
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.835
_diffrn_reflns_theta_min         2.359
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.489
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6490
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.0544 before and 0.0449 after correction.
The Ratio of minimum to maximum transmission is 0.8704.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_description       Chunk
_exptl_crystal_F_000             2712
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.047
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         7874
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0357P)^2^+15.6621P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0708
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7244
_reflns_number_total             7874
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b10888_si_002.cif
_cod_data_source_block           u_nhtripp_2
_cod_original_cell_volume        6638.9(8)
_cod_database_code               4133540
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.754
_shelx_estimated_absorpt_t_min   0.564
_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. Restrained distances
 C4S-C3S \\sim C3S-C2S \\sim C2S-C1S
 with sigma of 0.02
 O1S-C4S \\sim O1S-C1S
 with sigma of 0.02
 O1S-C3S \\sim O1S-C2S
 with sigma of 0.04
 C3S-C1S \\sim C4S-C2S
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O1S \\sim C4S \\sim C3S \\sim C2S \\sim C1S: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(C1S) = Uanis(C4S)
4. Rigid body (RIGU) restrains
 O1S, C4S, C3S, C2S, C1S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O1S(0.5) C4S(0.5) H4SA(0.5) H4SB(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5)
 C2S(0.5) H2SA(0.5) H2SB(0.5) C1S(0.5) H1SA(0.5) H1SB(0.5)
6.a Free rotating group:
 O1S(C4S,C3S,C2S,C1S)
6.b Ternary CH refined with riding coordinates:
 C19(H19), C16(H16), C13(H13), C33(H33), C27(H27), C30(H30)
6.c Secondary CH2 refined with riding coordinates:
 C4S(H4SA,H4SB), C3S(H3SA,H3SB), C2S(H2SA,H2SB), C1S(H1SA,H1SB)
6.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C11(H11), C24(H24), C5(H5), C9(H9), C26(H26), C4(H4)
6.e Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C17(H17A,H17B,
 H17C), C21(H21A,H21B,H21C), C34(H34A,H34B,H34C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C20(H20A,H20B,H20C), C31(H31A,H31B,H31C), C35(H35A,H35B,H35C),
 C32(H32A,H32B,H32C)
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_shelx_res_checksum              87351
_shelx_hkl_checksum              77249
_olex2_submission_special_instructions 'No special instructions were received'