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_4121734
_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            'C48 H108 K O16 Si4 U'
_chemical_formula_weight         1330.83
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.836(5)
_cell_angle_beta                 89.435(5)
_cell_angle_gamma                67.668(7)
_cell_formula_units_Z            2
_cell_length_a                   13.0129(10)
_cell_length_b                   13.9929(11)
_cell_length_c                   20.2901(11)
_cell_measurement_reflns_used    4391
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.9810
_cell_measurement_theta_min      3.5140
_cell_volume                     3416.8(5)
_computing_cell_refinement
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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)
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_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)
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_computing_data_reduction
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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_molecular_graphics
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Mercury 3.1 New software for searching the Cambridge Structural Database 
and visualizing crystal structures (I.J. Bruno, J.C. Cole, P.R. Edgington, 
M. Kessler, C.F. Macrae, P. McCabe, J. Pearson, R. Taylor, 
Acta Cryst., 2002, B58, 389-397)
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_computing_publication_material  'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement
;
OLEX2: a complete structure solution, refinement and analysis program 
(O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and 
H. Puschmann. J. Appl. Cryst. 2009, 42, 339-34).
;
_computing_structure_solution
;
SUPERFLIP program (Palatinus, L. & Chapuis, G. J. Appl. Cryst., 2007,
 40, 786-790)
;
_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  -39.00    3.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2801  -77.0000   90.0000 42

  2 omega  -56.00   42.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2801   77.0000  -30.0000 98

  3 omega  -88.00    4.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2801  -19.0000   30.0000 92

  4 omega  -71.00   -6.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2801  -77.0000   30.0000 65

  5 omega  -93.00    1.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2801  -77.0000 -150.0000 94

  6 omega  -96.00  -55.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2801  -57.0000  -90.0000 41

  7 omega  -49.00   42.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2801   57.0000 -180.0000 91

;
_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  0.0948
_diffrn_reflns_av_sigmaI/netI    0.1585
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30813
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.37
_exptl_absorpt_coefficient_mu    2.560
_exptl_absorpt_correction_T_max  0.9341
_exptl_absorpt_correction_T_min  0.2777
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'translucent dark red'
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1382
_exptl_crystal_size_max          0.67
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.640
_refine_diff_density_min         -2.287
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         13961
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1315
_refine_ls_R_factor_gt           0.0791
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0712P)^2^+1.4196P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1682
_refine_ls_wR_factor_ref         0.2036
_reflns_number_gt                8925
_reflns_number_total             13961
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5017624_si_002.cif
_cod_data_source_block           ojc31
_cod_depositor_comments
'Adding full bibliography for 4121734--4121736.cif.'
_cod_original_cell_volume        3416.8(4)
_cod_database_code               4121734