Multimetallic Cooperativity in Uranium-Mediated CO2 Activation.
Cooper, Oliver; Camp, Clément; Pécaut, Jacques; Kefalidis, Christos E.; Maron, Laurent; Gambarelli, Serge; Mazzanti, Marinella; Journal of the American Chemical Society 136 (2014) 6716–6723; doi:10.1021/ja5017624

data_4121736
_publ_section_title
;
 Multimetallic Cooperativity in Uranium-Mediated CO2 Activation.
;
_journal_issue                   18
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6716
_journal_page_last               6723
_journal_paper_doi               10.1021/ja5017624
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'C69.75 H142 K2 O25 Si4 U'
_chemical_formula_weight         1809.42
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 92.983(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.8819(9)
_cell_length_b                   16.4764(5)
_cell_length_c                   46.4053(12)
_cell_measurement_reflns_used    11436
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.4994
_cell_measurement_theta_min      3.3247
_cell_volume                     18998.7(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   -5.00   96.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   77.0000 -180.0000 101

  2 omega  -26.00   76.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051    0.0000   30.0000 102

  3 omega  -53.00    3.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239   37.0000  -60.0000 56

  4 omega  -47.00   50.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051  -37.0000  -90.0000 97

  5 omega  -22.00   -1.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051  -99.0000   60.0000 21

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_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  0.0867
_diffrn_reflns_av_sigmaI/netI    0.1183
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            63350
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.35
_exptl_absorpt_coefficient_mu    1.909
_exptl_absorpt_correction_T_max  0.7410
_exptl_absorpt_correction_T_min  0.4673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light violet'
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             7572
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.497
_refine_diff_density_min         -2.017
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.323
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1037
_refine_ls_number_reflns         19404
_refine_ls_number_restraints     202
_refine_ls_restrained_S_all      1.325
_refine_ls_R_factor_all          0.1468
_refine_ls_R_factor_gt           0.0983
_refine_ls_shift/su_max          0.052
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0223P)^2^+39.5330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1447
_refine_ls_wR_factor_ref         0.1608
_reflns_number_gt                13470
_reflns_number_total             19404
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5017624_si_004.cif
_cod_data_source_block           ccco2
_cod_depositor_comments
'Adding full bibliography for 4121734--4121736.cif.'
_cod_original_cell_volume        18998.8(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4121736