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_4108349
_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
;
 C79 H108 N4 O5 U, 1.375(C2 H3 N), 0.625(C4 H10 O)
;
_chemical_formula_sum            'C84.25 H118.38 N5.38 O5.63 U'
_chemical_formula_weight         1534.50
_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                 96.82(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.970(3)
_cell_length_b                   24.531(4)
_cell_length_c                   20.930(2)
_cell_measurement_reflns_used    422
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      6.00
_cell_volume                     7632(2)
_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      100(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 1.30 \% and 117 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  0.1057
_diffrn_reflns_av_sigmaI/netI    0.0872
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            102321
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         3.36
_exptl_absorpt_coefficient_mu    2.182
_exptl_absorpt_correction_T_max  0.822
_exptl_absorpt_correction_T_min  0.641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       prism
_exptl_crystal_F_000             3194
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.147
_refine_diff_density_min         -1.614
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     916
_refine_ls_number_reflns         16810
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0330P)^2^+21.3866P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.1004
_reflns_number_gt                11825
_reflns_number_total             16810
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja804263w_si_006.cif
_cod_data_source_block           sd0729
_cod_original_sg_symbol_Hall     -P2ybc
_cod_database_code               4108349