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_4118412
_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         'C115 H140 N2 O6 U2, 2(C4 H10 O2)'
_chemical_formula_sum            'C123 H160 N2 O10 U2'
_chemical_formula_weight         2302.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_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                 109.604(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.114(3)
_cell_length_b                   18.5122(18)
_cell_length_c                   21.760(2)
_cell_measurement_reflns_used    9880
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.57
_cell_measurement_theta_min      2.31
_cell_volume                     10668.6(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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      100(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Quazar focussing montel optics'
_diffrn_radiation_source         'ImuS micro-focus tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_sigmaI/netI    0.0434
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            97532
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    3.092
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2009'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       plate
_exptl_crystal_F_000             4704
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.633
_refine_diff_density_min         -1.599
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.874
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1519
_refine_ls_number_reflns         23528
_refine_ls_number_restraints     361
_refine_ls_restrained_S_all      1.885
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0081P)^2^+6.0561P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0863
_reflns_number_gt                19861
_reflns_number_total             23528
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3047393_3.cif
_cod_data_source_block           bk1110
_cod_original_cell_volume        10668.5(18)
_cod_original_sg_symbol_Hall     -P2ybc
_cod_database_code               4118412