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_4337917
_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         'C51 H58 N3 O2 U1'
_chemical_formula_sum            'C51 H58 N3 O2 U'
_chemical_formula_weight         983.03
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 94.776(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5323(3)
_cell_length_b                   12.9693(3)
_cell_length_c                   29.1811(6)
_cell_measurement_reflns_used    37135
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      72.249
_cell_measurement_theta_min      3.732
_cell_volume                     4349.34(18)
_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 0.979
_diffrn_measured_fraction_theta_max 0.958
_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  0.050
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            37135
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.249
_diffrn_reflns_theta_min         3.732
_diffrn_source                   'microfocus source'
_exptl_absorpt_coefficient_mu    10.829
_exptl_absorpt_correction_T_max  0.522
_exptl_absorpt_correction_T_min  0.017
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_description       block
_exptl_crystal_F_000             1972
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.810
_refine_diff_density_min         -1.193
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         8221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0535P)^2^+9.9515P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0881
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7617
_reflns_number_total             8221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic500012x_si_001.cif
_cod_data_source_block           JK5100
_cod_depositor_comments
'Adding full bibliography for 4337916--4337924.cif.'
_cod_database_code               4337917
_shelx_estimated_absorpt_t_min   0.411
_shelx_estimated_absorpt_t_max   0.563
_shelxl_version_number           2013-3
_shelx_res_checksum              74575
_shelx_hkl_checksum
'9956 CheckCif Response No level A or B alerts have been detected.'