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_4133541
_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 N2 U, C32 H12 B F24, 0.25(C4 H10 O)'
_chemical_formula_sum            'C105 H114.5 B F24 N2 O0.25 U'
_chemical_formula_weight         2113.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-06-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.8930(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7775(2)
_cell_length_b                   16.4035(2)
_cell_length_c                   41.8881(6)
_cell_measurement_reflns_used    9984
_cell_measurement_temperature    172.98
_cell_measurement_theta_max      72.025
_cell_measurement_theta_min      2.893
_cell_volume                     10152.6(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'COSMO (BRUKER, V1.61, 2009)'
_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
'SHELXS (Sheldrick, Acta Cryst. A64 2008, 112-122)'
_diffrn_ambient_temperature      172.98
_diffrn_detector_area_resol_mean 8.4
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1307
_diffrn_reflns_av_unetI/netI     0.0952
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            78623
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.132
_diffrn_reflns_theta_min         2.110
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.277
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.4605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1052 before and 0.0775 after correction.
The Ratio of minimum to maximum transmission is 0.6111.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_description       Block
_exptl_crystal_F_000             4294
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.062
_refine_diff_density_max         1.395
_refine_diff_density_min         -1.232
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1530
_refine_ls_number_reflns         19461
_refine_ls_number_restraints     934
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0644P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1415
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13327
_reflns_number_total             19461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b10888_si_002.cif
_cod_data_source_block           unhtripp2barf
_cod_original_formula_sum        'C105 H114.50 B F24 N2 O0.25 U'
_cod_database_code               4133541
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.736
_shelx_estimated_absorpt_t_min   0.343
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F9A-F7A \\sim F9A-F8A \\sim F7A-F8A \\sim F9-F8 \\sim F9-F7 \\sim F8-F7
 with sigma of 0.04
 C87-C83 \\sim C87-F9A \\sim C87-F7A \\sim C87-F8A \\sim C87-F9 \\sim C87-F8
\\sim C87-F7
 with sigma of 0.02
 F10A-F11A \\sim F10A-F12A \\sim F11A-F12A \\sim F10-F12 \\sim F10-F11 \\sim
F12-F11
 with sigma of 0.04
 C88-F10A \\sim C88-F11A \\sim C88-F12A \\sim C88-C85 \\sim C88-F10 \\sim
C88-F12 \\sim C88-F11
 with sigma of 0.02
 F5-F4 \\sim F5-F6 \\sim F4-F6 \\sim F6A-F5A \\sim F6A-F4A \\sim F5A-F4A
 with sigma of 0.04
 C80-F5 \\sim C80-C77 \\sim C80-F4 \\sim C80-F6 \\sim C80-F6A \\sim C80-F5A
\\sim C80-F4A
 with sigma of 0.02
 F22A-F23A \\sim F23A-F24A \\sim F23-F22 \\sim F23-F24 \\sim F22-F24
 with sigma of 0.04
 C103-F22A \\sim C103-F23A \\sim C103-F24A \\sim C103-C101 \\sim C103-F23 \\sim
C103-F22 \\sim C103-F24
 with sigma of 0.02
 F18A-F16A \\sim F18A-F17A \\sim F16A-F17A \\sim F16-F18 \\sim F16-F17
 with sigma of 0.04
 C96-F18A \\sim C96-F16A \\sim C96-F17A \\sim C96-C93 \\sim C96-F16 \\sim
C96-F18 \\sim C96-F17
 with sigma of 0.02
 F13-F14 \\sim F13-F15 \\sim F14-F15 \\sim F15A-F14A \\sim F15A-F13A \\sim
F14A-F13A
 with sigma of 0.04
 C95-F13 \\sim C95-F14 \\sim C95-F15 \\sim C95-C91 \\sim C95-F15A \\sim
C95-F14A \\sim C95-F13A
 with sigma of 0.02
 F2A-F1A \\sim F2A-F3A \\sim F1A-F3A \\sim F3-F2 \\sim F3-F1 \\sim F2-F1
 with sigma of 0.04
 C79-F2A \\sim C79-F1A \\sim C79-F3A \\sim C79-C75 \\sim C79-F3 \\sim C79-F2
\\sim C79-F1
 with sigma of 0.02
 F21-F19 \\sim F21-F20 \\sim F19-F20 \\sim F21A-F19A \\sim F20A-F19A
 with sigma of 0.04
 C104-F21 \\sim C104-F19 \\sim C104-F20 \\sim C104-C99 \\sim C104-F21A \\sim
C104-F20A \\sim C104-F19A
 with sigma of 0.02
 C16-C17 \\sim C16-C10 \\sim C16-C18 \\sim C16-C18A \\sim C16-C17A
 with sigma of 0.02
 C61-C68 \\sim C61-C69 \\sim C68-C69 \\sim C68-C68A \\sim C69-C68A
 with sigma of 0.04
 C67-C61 \\sim C67-C68 \\sim C67-C69 \\sim C67-C68A
 with sigma of 0.02
 C66-C65 \\sim C65A-C66A
 with sigma of 0.04
 C64-C66 \\sim C64-C59 \\sim C64-C65 \\sim C64-C65A \\sim C64-C66A
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 F9A, F7A, F8A, C87, C83
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F9, F8, F7, C87, C83
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F11A, C88, F12A, F10A, C85
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F10, F12, C88, F11, C85
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C80, C77, F5, F6, F4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C80, F4A, F6A, C77, F5A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C103, F22A, F24A, F23A, C101
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F22, F23, F24, C103, C101
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C96, F17A, F16A, F18A, C93
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C96, C93, F18, F16, F17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C91, F14, F13, F15, C95
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C91, C95, F14A, F15A, F13A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1A, C75, C79, F3A, F2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C75, C79, F3, F2, F1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C104, C99, F19, F20, F21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F20A, C104, F21A, F19A, C99
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C61
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C17A, C16, C18A, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C18, C16, C17, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C61, C67, C68, C68A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C61, C67, C68, C69
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C4S, C3S, C2S, C1S, O1S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C59, C64, C65, C66
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C59, C64, C65A, C66A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C25, C31, C32, C33
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1, C6, C5, C4, C3, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: F2A(0.51109) F18A(0.80812) F16A(0.80812) F21(0.60504) F1A(0.51109)
 F22A(0.74515) F23A(0.74515) F3A(0.51109) F13(0.77559) F19(0.60504)
 F20(0.60504) F14(0.77559) F15(0.77559) F17A(0.80812) F10A(0.59068)
 F11A(0.59068) F12A(0.59068) F5(0.62763) C17(0.58) H17A(0.58) H17B(0.58)
 H17C(0.58) F9A(0.5115) H64(0.67) H64A(0.33) C18(0.58) H18A(0.58) H18B(0.58)
 H18C(0.58) C66(0.67) H66A(0.67) H66B(0.67) H66C(0.67) F4(0.62763)
 F24A(0.74515) F7A(0.5115) F8A(0.5115) H16(0.58) H16A(0.42) F6(0.62763)
 C65(0.67) H65A(0.67) H65B(0.67) H65C(0.67) F9(0.4885) F8(0.4885) F7(0.4885)
 F10(0.40932) F12(0.40932) F11(0.40932) F6A(0.37237) F5A(0.37237) F4A(0.37237)
 F23(0.25485) F22(0.25485) F24(0.25485) F16(0.19188) F18(0.19188) F17(0.19188)
 F15A(0.22441) F14A(0.22441) F13A(0.22441) F3(0.48891) F2(0.48891) F1(0.48891)
 F21A(0.39496) F20A(0.39496) F19A(0.39496) C18A(0.42) H18D(0.42) H18E(0.42)
 H18F(0.42) C17A(0.42) H17D(0.42) H17E(0.42) H17F(0.42) H67(0.68) H67A(0.32)
 C69(0.68) H69A(0.68) H69B(0.68) H69C(0.68) C68A(0.32) H68D(0.32) H68E(0.32)
 H68F(0.32) O1S(0.25) C3S(0.25) H3SA(0.25) H3SB(0.25) C2S(0.25) H2SA(0.25)
 H2SB(0.25) C1S(0.25) H1SA(0.25) H1SB(0.25) H1SC(0.25) C4S(0.25) H4SA(0.25)
 H4SB(0.25) H4SC(0.25) C65A(0.33) H65D(0.33) H65E(0.33) H65F(0.33) C66A(0.33)
 H66D(0.33) H66E(0.33) H66F(0.33)
5.a Ternary CH refined with riding coordinates:
 C70(H70), C64(H64), C64(H64A), C16(H16), C16(H16A), C55(H55), C13(H13),
 C49(H49), C52(H52), C19(H19), C67(H67), C67(H67A), C34(H34), C28(H28), C31(H31)
5.b Secondary CH2 refined with riding coordinates:
 C3S(H3SA,H3SB), C2S(H2SA,H2SB)
5.c Aromatic/amide H refined with riding coordinates:
 C78(H78), C9(H9), C39(H39), N1(H1), C41(H41), C11(H11), C84(H84), C40(H40),
 C102(H102), C62(H62), C100(H100), C94(H94), C90(H90), C98(H98), C74(H74),
 C92(H92), C60(H60), C82(H82), C86(H86), C76(H76), C45(H45), C47(H47), C26(H26),
  C3(H3), C4(H4), C24(H24), C5(H5)
5.d Idealised Me refined as rotating group:
 C51(H51A,H51B,H51C), C15(H15A,H15B,H15C), C54(H54A,H54B,H54C), C21(H21A,H21B,
 H21C), C53(H53A,H53B,H53C), C56(H56A,H56B,H56C), C14(H14A,H14B,H14C), C20(H20A,
 H20B,H20C), C57(H57A,H57B,H57C), C50(H50A,H50B,H50C), C71(H71A,H71B,H71C),
 C72(H72A,H72B,H72C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C66(H66A,H66B,
 H66C), C65(H65A,H65B,H65C), C18A(H18D,H18E,H18F), C17A(H17D,H17E,H17F),
 C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C68A(H68D,H68E,H68F), C1S(H1SA,H1SB,
 H1SC), C4S(H4SA,H4SB,H4SC), C65A(H65D,H65E,H65F), C66A(H66D,H66E,H66F),
 C36(H36A,H36B,H36C), C35(H35A,H35B,H35C), C30(H30A,H30B,H30C), C29(H29A,H29B,
 H29C), C33(H33A,H33B,H33C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              84853
_shelx_hkl_checksum              96776
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'