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_4337918
_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_formula_moiety
;
;
_chemical_formula_sum            'C58.5 H68.5 I N3 O2 U'
_chemical_formula_weight         1210.59
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                72.608(2)
_cell_angle_beta                 73.288(2)
_cell_angle_gamma                65.8220(10)
_cell_formula_units_Z            2
_cell_length_a                   12.8518(3)
_cell_length_b                   15.4726(5)
_cell_length_c                   15.6750(6)
_cell_measurement_reflns_used    36605
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      30.493
_cell_measurement_theta_min      1.803
_cell_volume                     2664.29(15)
_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    'SHELXT (Sheldrick)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.044
_diffrn_reflns_av_unetI/netI     0.0606
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36605
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.493
_diffrn_reflns_theta_min         1.803
_diffrn_source                   'microfocus source'
_exptl_absorpt_coefficient_mu    3.668
_exptl_absorpt_correction_T_max  0.172
_exptl_absorpt_correction_T_min  0.163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1203
_exptl_crystal_size_max          0.720
_exptl_crystal_size_mid          0.600
_exptl_crystal_size_min          0.480
_refine_diff_density_max         6.928
_refine_diff_density_min         -1.901
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         16047
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0549
_refine_ls_shift/su_max          0.094
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0814P)^2^+4.8223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1363
_refine_ls_wR_factor_ref         0.1483
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12308
_reflns_number_total             16047
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic500012x_si_001.cif
_cod_data_source_block           JK4201
_cod_depositor_comments
'Adding full bibliography for 4337916--4337924.cif.'
_cod_original_formula_sum        'C58.50 H68.50 I N3 O2 U'
_cod_database_code               4337918
_shelx_estimated_absorpt_t_min   0.178
_shelx_estimated_absorpt_t_max   0.272
_shelxl_version_number           2013-3
_shelx_res_checksum              25614
_shelx_hkl_checksum              25057
_shelx_fab_checksum
'54997 CheckCif Responses PLAT330 Alert 2 A: C921-C926 belong to an outer sphere toluene. The outer sphere solvents in this molecule show significant disorder. These have no bearing on the compound of interest. PLAT221 Alert 2 B: See above explanation. PLAT223 Alert 4 B: See above explanation.'