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_4133542
_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, C6 H14'
_chemical_formula_sum            'C78 H114 I N2 U'
_chemical_formula_weight         1444.64
_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                 94.3230(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3008(15)
_cell_length_b                   15.0013(17)
_cell_length_c                   36.190(4)
_cell_measurement_reflns_used    9799
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.997
_cell_measurement_theta_min      2.370
_cell_volume                     7200.4(14)
_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      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0470
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            80270
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.157
_diffrn_reflns_theta_min         2.370
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.724
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6038
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.0787 before and 0.0480 after correction. The Ratio of minimum to maximum transmission is 0.8099. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       Hexagonal
_exptl_crystal_F_000             2964
_exptl_crystal_recrystallization_method
'The material was recrystallised from hexane by cooling a concentrated solution to -35 C'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.703
_refine_diff_density_min         -0.850
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     743
_refine_ls_number_reflns         15912
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+15.8596P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0813
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13377
_reflns_number_total             15912
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b10888_si_002.cif
_cod_data_source_block           trippnh2ui_hexane
_cod_database_code               4133542
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.832
_shelx_estimated_absorpt_t_min   0.586
_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
 C1A-C1B \\sim C1B-C1C \\sim C1C-C1D \\sim C1D-C1E \\sim C1E-C1F
 with sigma of 0.02
 C1A-C1C \\sim C1C-C1E \\sim C1B-C1D \\sim C1D-C1F
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C1A \\sim C1B \\sim C1C \\sim C1D \\sim C1E \\sim C1F: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
4.a Ternary CH refined with riding coordinates:
 C55(H55), C52(H52), C49(H49), C70(H70), C64(H64), C67(H67), C31(H31),
 C34(H34), C28(H28), C16(H16), C19(H19), C13(H13)
4.b Secondary CH2 refined with riding coordinates:
 C1B(H1BA,H1BB), C1C(H1CA,H1CB), C1D(H1DA,H1DB), C1E(H1EA,H1EB)
4.c Aromatic/amide H refined with riding coordinates:
 C47(H47), C45(H45), C39(H39), C40(H40), C41(H41), C62(H62), C60(H60), C3(H3),
 C4(H4), C5(H5), C24(H24), C26(H26), C9(H9), C11(H11)
4.d Idealised Me refined as rotating group:
 C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C53(H53A,H53B,H53C), C54(H54A,H54B,
 H54C), C51(H51A,H51B,H51C), C50(H50A,H50B,H50C), C72(H72A,H72B,H72C), C71(H71A,
 H71B,H71C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C69(H69A,H69B,H69C),
 C68(H68A,H68B,H68C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C36(H36A,H36B,
 H36C), C35(H35A,H35B,H35C), C30(H30A,H30B,H30C), C29(H29A,H29B,H29C), C17(H17A,
 H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C),
 C15(H15A,H15B,H15C), C14(H14A,H14B,H14C), C1A(H1AA,H1AB,H1AC), C1F(H1FA,H1FB,
 H1FC)
;
_shelx_res_checksum              30117
_shelx_hkl_checksum              76264
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a glass fibre in paratone oil'
_olex2_submission_special_instructions 'No special instructions were received'