Carbon Dioxide Activation with Sterically Pressured Mid- and High-Valent Uranium Complexes
Suzanne C. Bart; Christian Anthon; Frank W. Heinemann; Eckhard Bill; Norman M. Edelstein; Karsten Meyer; Journal of the American Chemical Society 130 (2008) 12536–12546; doi:10.1021/ja804263w

data_4108350
_publ_section_title
;
 Carbon Dioxide Activation with Sterically Pressured Mid- and High-Valent
 Uranium Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12536
_journal_page_last               12546
_journal_paper_doi               10.1021/ja804263w
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C61 H90 N4 O5 U, 2(C4 H10 O)'
_chemical_formula_sum            'C69 H110 N4 O7 U'
_chemical_formula_weight         1345.64
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.49(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.342(2)
_cell_length_b                   17.744(1)
_cell_length_c                   26.201(3)
_cell_measurement_reflns_used    677
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      6.00
_cell_volume                     7110.8(13)
_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      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
;
 \f- and \w-rotations with 1.10 \% and 55 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  0.0711
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            198703
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    2.333
_exptl_absorpt_correction_T_max  0.660
_exptl_absorpt_correction_T_min  0.579
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_description       prism
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.264
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     756
_refine_ls_number_reflns         16937
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+9.4008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0718
_refine_ls_wR_factor_ref         0.0817
_reflns_number_gt                12661
_reflns_number_total             16937
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja804263w_si_007.cif
_cod_data_source_block           sd0742
_cod_original_sg_symbol_Hall     -P2yn
_cod_database_code               4108350