Synthesis and Reactivity of a U(IV) Dibenzyne Complex
Pedrick, Elizabeth A.; Seaman, Lani A.; Scott, Joshua C.; Griego, Leonel; Wu, Guang; Hayton, Trevor W.; Organometallics 35 (2016) 494–; doi:10.1021/acs.organomet.5b00929

data_4088206
_publ_section_title
;
 Synthesis and Reactivity of a U(IV) Dibenzyne Complex
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              494
_journal_paper_doi               10.1021/acs.organomet.5b00929
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C44 H62 Li2 N4 O2 U'
_chemical_formula_weight         930.89
_chemical_name_systematic
; 
U(IV) cis benzyne 
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.009(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.494(5)
_cell_length_b                   10.946(2)
_cell_length_c                   18.895(4)
_cell_measurement_reflns_used    619
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.0255
_cell_measurement_theta_min      23.875
_cell_volume                     4203.1(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0917
_diffrn_reflns_av_sigmaI/netI    0.1272
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            26296
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.00
_exptl_absorpt_coefficient_mu    3.901
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6505
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.665
_refine_diff_density_min         -1.737
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         8565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.100
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0156P)^2^+4.7408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0614
_refine_ls_wR_factor_ref         0.0765
_reflns_number_gt                5438
_reflns_number_total             8565
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00929_si_002.cif
_cod_data_source_block           complex_2
_cod_original_cell_volume        4203.0(15)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4088206