Multielectron C-O Bond Activation Mediated by a Family of Reduced Uranium Complexes.
Kiernicki, John J.; Newell, Brian S.; Matson, Ellen M.; Anderson, Nickolas H.; Fanwick, Phillip E.; Shores, Matthew P.; Bart, Suzanne C.; Inorganic chemistry 53 (2014) 3730–; doi:10.1021/ic500012x

data_4337924
_publ_section_title
;
 Multielectron C-O Bond Activation Mediated by a Family of Reduced Uranium
 Complexes.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3730
_journal_paper_doi               10.1021/ic500012x
_journal_volume                  53
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C26 H39 I2 O3 U1'
_chemical_formula_sum            'C26 H39 I2 O3 U'
_chemical_formula_weight         891.40
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           45
_space_group_name_Hall           'I 2 -2c'
_space_group_name_H-M_alt        'I b a 2'
_symmetry_space_group_name_Hall  'I 2 -2c'
_symmetry_space_group_name_H-M   'I b a 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.2642(12)
_cell_length_b                   24.4304(10)
_cell_length_c                   12.2650(6)
_cell_measurement_reflns_used    13343
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.282
_cell_measurement_theta_min      2.685
_cell_volume                     6671.2(6)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Crystal Clear(Rigaku 2001)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR2004 (Burla, et. al., 2005)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_details
;
Data were collected on a Rigaku Rapid which has a quarter 
chi circle and a 200 degree curved image plate at a fixed 
distance of 127.4mm.  Strategy was optimized using the 
CrystalClear software.  The completeness is the best 
that can be obtained with this geometry. The missing data are not 
cusp data but mostly high angle data.
Also the use of HKL2000/SCALEPACK lowers the number 
of observed data as inconsistent equivalents are removed 
from the data set and not included in the collected total.
;
_diffrn_measurement_device_type  'Rigaku Rapid II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.098
_diffrn_reflns_av_unetI/netI     0.0589
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            13343
_diffrn_reflns_point_group_measured_fraction_full 0.739
_diffrn_reflns_point_group_measured_fraction_max 0.708
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.282
_diffrn_reflns_theta_min         2.685
_diffrn_source                   'microfocus source'
_exptl_absorpt_coefficient_mu    28.382
_exptl_absorpt_correction_T_max  0.182
_exptl_absorpt_correction_T_min  0.010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3336
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.060
_platon_squeeze_details
;
;
_refine_diff_density_max         1.974
_refine_diff_density_min         -2.412
_refine_diff_density_rms         0.221
_refine_ls_abs_structure_details
;
 Flack x determined using 1308 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         4664
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0652
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1219P)^2^+45.7707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1922
_refine_ls_wR_factor_ref         0.1947
_reflns_Friedel_coverage         0.451
_reflns_Friedel_fraction_full    0.497
_reflns_Friedel_fraction_max     0.464
_reflns_number_gt                4425
_reflns_number_total             4664
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic500012x_si_001.cif
_cod_data_source_block           EMM41
_cod_depositor_comments
'Adding full bibliography for 4337916--4337924.cif.'
_cod_database_code               4337924
_shelx_estimated_absorpt_t_min   0.070
_shelx_estimated_absorpt_t_max   0.281
_shelxl_version_number           2013-4
_shelx_res_checksum              85890
_shelx_hkl_checksum
'38777 CheckCif Response PLAT213 Alert 2 A: C2 is part of rotating cyclopentadienyl ring. Disorder is expected. PLAT029 Alert 3 A: Small crystal, insignificant amount of data not collected PLAT241 Alert 2 B: Disorder arrising from a coordinated solvent (bowtie-boat exchange) PLAT342 Alert 3 B: Only C-C bonds are Solvents and cyclopentadienyl ligand. Both are very active and result in larger than normal disorder.'