Insights into the mechanism of carbonate formation through reductive cleavage of carbon dioxide with low-valent uranium centers
Lam, Oanh P.; Bart, Suzanne C.; Kameo, Hajime; Heinemann, Frank W.; Meyer, Karsten; Chemical Communications 46 (2010) 3137–3139; doi:10.1039/b927142b

data_7105504
_publ_section_title
;
 Insights into the mechanism of carbonate formation through reductive
 cleavage of carbon dioxide with low-valent uranium centers
;
_journal_issue                   18
_journal_name_full               'Chemical Communications'
_journal_page_first              3137
_journal_page_last               3139
_journal_paper_doi               10.1039/b927142b
_journal_volume                  46
_journal_year                    2010
_chemical_formula_moiety         'C109 H150 O9 U2, C7 H8, 1.5(C4 H10 O)'
_chemical_formula_sum            'C122 H173 O10.5 U2'
_chemical_formula_weight         2283.66
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.4828(18)
_cell_length_b                   25.766(2)
_cell_length_c                   25.784(2)
_cell_measurement_reflns_used    399
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      6.00
_cell_volume                     11614.7(17)
_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      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
;
\f- and \w-rotations with 1.20 \% and 360 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  0.0818
_diffrn_reflns_av_sigmaI/netI    0.1025
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            116536
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         3.16
_exptl_absorpt_coefficient_mu    2.840
_exptl_absorpt_correction_T_max  0.843
_exptl_absorpt_correction_T_min  0.572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4692
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.339
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details
;
Flack H D (1983), Acta Cryst. A39, 876-881
11461 Friedel pairs used in the refinement of Flack parameter
;
_refine_ls_abs_structure_Flack   0.011(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1278
_refine_ls_number_reflns         25130
_refine_ls_number_restraints     193
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0305P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0798
_reflns_number_gt                18640
_reflns_number_total             25130
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b927142b.txt
_cod_data_source_block           sd0803a
_cod_original_sg_symbol_Hall     P2ac2ab
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_original_formula_sum        'C122 H173 O10.50 U2'
_cod_database_code               7105504