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_4110782
_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         'C39 H69 O Si2 U'
_chemical_formula_sum            'C39 H69 O Si2 U'
_chemical_formula_weight         848.15
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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             2006-04-04T10:50:18-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90.652(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8533(2)
_cell_length_b                   14.8390(2)
_cell_length_c                   22.5090(3)
_cell_measurement_reflns_used    45751
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     3958.88(10)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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      0.340156E-1
_diffrn_orient_matrix_UB_12      0.50741E-2
_diffrn_orient_matrix_UB_13      -0.403142E-1
_diffrn_orient_matrix_UB_21      -0.556911E-1
_diffrn_orient_matrix_UB_22      -0.449051E-1
_diffrn_orient_matrix_UB_23      -0.157414E-1
_diffrn_orient_matrix_UB_31      -0.534767E-1
_diffrn_orient_matrix_UB_32      0.49992E-1
_diffrn_orient_matrix_UB_33      -0.100478E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.073
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            58842
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         3.44
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    4.187
_exptl_absorpt_correction_T_max  0.6615
_exptl_absorpt_correction_T_min  0.5300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       needle
_exptl_crystal_F_000             1724
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.156
_refine_diff_density_min         -1.169
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         7771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0344P)^2^+16.1434P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                6512
_reflns_number_total             7771
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja063222rsi20060613_122836.cif
_cod_data_source_block           apr206
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4110782