Uranium(III)-Mediated C-C-Coupling of Terminal Alkynes: Formation of Dinuclear Uranium(IV) Vinyl Complexes
Boris Kosog; Christos E. Kefalidis; Frank W. Heinemann; Laurent Maron; Karsten Meyer; Journal of the American Chemical Society 134 (2012) 12792–12797; doi:10.1021/ja3047393

data_4118413
_publ_contact_author
;                                                                               
        Prof. Dr. K. Meyer       
        Department of Chemistry and Pharmacy
        Inorganic Chemistry
        Universit\"at Erlangen-N\"urnberg                   
        Egerlandstr. 1                                     
        D-91058 Erlangen                               
        Bundesrepublik Deutschland                             
;
_publ_contact_author_email       Karsten.Meyer@chemie.uni-erlangen.de
_publ_contact_author_fax         '049 9131 852-7367'
_publ_contact_author_phone       '049 9131 852-7360'
_publ_section_title
;
 Uranium(III)-Mediated C-C-Coupling of Terminal Alkynes: Formation of
 Dinuclear Uranium(IV) Vinyl Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12792
_journal_page_last               12797
_journal_paper_doi               10.1021/ja3047393
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C120 H152 N2 O6 U2, C4 H10 O2'
_chemical_formula_sum            'C124 H162 N2 O8 U2'
_chemical_formula_weight         2284.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.031(5)
_cell_angle_beta                 101.942(9)
_cell_angle_gamma                91.137(8)
_cell_formula_units_Z            2
_cell_length_a                   15.308(2)
_cell_length_b                   16.2270(8)
_cell_length_c                   22.224(3)
_cell_measurement_reflns_used    379
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      6.00
_cell_volume                     5270.9(10)
_computing_cell_refinement       'EVALCCD (Duisenberg, 2003)'
_computing_data_collection       'COLLECT (Bruker-Nonius, 2002)'
_computing_data_reduction        'EVALCCD (Duisenberg, 2003)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_refinement  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
;
 \f- and \w-rotations with 1.50 \% and 75 sec per frame
;
_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  0.0868
_diffrn_reflns_av_sigmaI/netI    0.0621
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            161847
_diffrn_reflns_theta_full        29.50
_diffrn_reflns_theta_max         29.50
_diffrn_reflns_theta_min         5.80
_exptl_absorpt_coefficient_mu    3.128
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       prism
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.478
_refine_diff_density_min         -1.365
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1288
_refine_ls_number_reflns         29117
_refine_ls_number_restraints     89
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0244P)^2^+9.2023P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0802
_reflns_number_gt                21474
_reflns_number_total             29117
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3047393_4.cif
_cod_data_source_block           bk1114
_cod_original_cell_volume        5270.9(11)
_cod_original_sg_symbol_Hall     -P1
_cod_database_code               4118413