Mechanistic Studies on the Reductive Cyclooligomerisation of CO by U(III) Mixed Sandwich Complexes; the Molecular Structure of [(U(η-C8H6{SiiPr3-1,4}2)(η-Cp*)]2(μ-η1:η1-C2O2)
Alistair S. Frey; F. Geoffrey N. Cloke; Peter B. Hitchcock; Iain J. Day; Jennifer C. Green; Georgina Aitken; Journal of the American Chemical Society 130 (2008) 13816–13817; doi:10.1021/ja8059792

data_4108522
_publ_section_title
;
 Mechanistic Studies on the Reductive Cyclooligomerisation of CO by U(III)
 Mixed Sandwich Complexes; the Molecular Structure of
 [(U(\h-C8H6{SiiPr3-1,4}2)(\h-Cp*)]2(\m-\h1:\h1-C2O2)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13816
_journal_page_last               13817
_journal_paper_doi               10.1021/ja8059792
_journal_volume                  130
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C74 H126 O2 Si4 U2, 2(C5 H12 O)'
_chemical_formula_sum            'C84 H150 O4 Si4 U2'
_chemical_formula_weight         1812.46
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2008-03-10T10:30:26-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.4419(2)
_cell_length_b                   24.1793(3)
_cell_length_c                   51.1378(7)
_cell_measurement_reflns_used    523307
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     17857.1(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.681783E-1
_diffrn_orient_matrix_UB_12      -0.71741E-2
_diffrn_orient_matrix_UB_13      0.4027E-3
_diffrn_orient_matrix_UB_21      -0.21768E-2
_diffrn_orient_matrix_UB_22      0.24817E-2
_diffrn_orient_matrix_UB_23      -0.195101E-1
_diffrn_orient_matrix_UB_31      0.11898E-1
_diffrn_orient_matrix_UB_32      -0.40655E-1
_diffrn_orient_matrix_UB_33      -0.1262E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0714
_diffrn_reflns_av_unetI/netI     0.038
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       62
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            125507
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         3.46
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    3.72
_exptl_absorpt_correction_T_max  0.4916
_exptl_absorpt_correction_T_min  0.3733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_description       prism
_exptl_crystal_F_000             7408
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.742
_refine_diff_density_min         -1.32
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.306
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     810
_refine_ls_number_reflns         17331
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.307
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0645
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+185.4209P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1302
_reflns_number_gt                15000
_reflns_number_total             17331
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8059792_si_001.cif
_cod_data_source_block           mar608
_cod_database_code               4108522