Reductive Cyclotetramerization of CO to Squarate by a U(III) Complex: The X-ray Crystal Structure of [(U(η-C8H6{SiiPr3-1,4}2)(η-C5Me4H)]2(μ-η2:η2-C4O4)
Owen T. Summerscales; F. Geoffrey N. Cloke; Peter B. Hitchcock; Jennifer C. Green; Nilay Hazari; Journal of the American Chemical Society 128 (2006) 9602–9603; doi:10.1021/ja063222r

data_4110783
_publ_section_title
;
 Reductive Cyclotetramerization of CO to Squarate by a U(III) Complex: The
 X-ray Crystal Structure of
 [(U(\h-C8H6{SiiPr3-1,4}2)(\h-C5Me4H)]2(\m-\h2:\h2-C4O4)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9602
_journal_page_last               9603
_journal_paper_doi               10.1021/ja063222r
_journal_volume                  128
_journal_year                    2006
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C74 H122 O4 Si4 U2, C4 H10 O'
_chemical_formula_sum            'C78 H132 O5 Si4 U2'
_chemical_formula_weight         1738.26
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2006-03-15T09:59:23-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                68.152(3)
_cell_angle_beta                 74.018(3)
_cell_angle_gamma                73.408(2)
_cell_formula_units_Z            1
_cell_length_a                   10.9003(5)
_cell_length_b                   13.6373(7)
_cell_length_c                   15.7777(6)
_cell_measurement_reflns_used    53329
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     2048.24(17)
_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-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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      0.298051E-1
_diffrn_orient_matrix_UB_12      0.697535E-1
_diffrn_orient_matrix_UB_13      -0.218537E-1
_diffrn_orient_matrix_UB_21      -0.191266E-1
_diffrn_orient_matrix_UB_22      0.1874E-3
_diffrn_orient_matrix_UB_23      0.656785E-1
_diffrn_orient_matrix_UB_31      0.908447E-1
_diffrn_orient_matrix_UB_32      -0.406224E-1
_diffrn_orient_matrix_UB_33      0.68099E-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  0.1275
_diffrn_reflns_av_unetI/netI     0.0832
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30905
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.47
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    4.051
_exptl_absorpt_correction_T_max  0.9254
_exptl_absorpt_correction_T_min  0.5719
_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    1.409
_exptl_crystal_description       plate
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.619
_refine_diff_density_min         -2.74
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         7927
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0663P)^2^+8.8566P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1416
_reflns_number_gt                6679
_reflns_number_total             7927
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja063222rsi20060613_122901.cif
_cod_data_source_block           mar1306
_cod_original_cell_volume        2048.24(16)
_cod_database_code               4110783