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_4337921
_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 unk
_chemical_formula_moiety         'C37 H46 I1 N3 U1'
_chemical_formula_sum            'C37 H46 I N3 U'
_chemical_formula_weight         897.70
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.9579(7)
_cell_length_b                   12.3690(3)
_cell_length_c                   11.8789(2)
_cell_measurement_reflns_used    21292
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.022
_cell_measurement_theta_min      2.235
_cell_volume                     3960.93(16)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Nonius Collect (Nonius, 1998)'
_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 0.891
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.077
_diffrn_reflns_av_unetI/netI     0.1004
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            21292
_diffrn_reflns_point_group_measured_fraction_full 0.895
_diffrn_reflns_point_group_measured_fraction_max 0.738
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.022
_diffrn_reflns_theta_min         2.235
_diffrn_source                   'fine focus tube'
_exptl_absorpt_coefficient_mu    4.902
_exptl_absorpt_correction_T_max  0.676
_exptl_absorpt_correction_T_min  0.069
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       plate
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.596
_refine_diff_density_min         -1.837
_refine_diff_density_rms         0.132
_refine_ls_abs_structure_details
;
 Flack x determined using 1607 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.079(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         7807
_refine_ls_number_restraints     166
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.065
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0055P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0676
_reflns_Friedel_coverage         0.584
_reflns_Friedel_fraction_full    0.778
_reflns_Friedel_fraction_max     0.570
_reflns_number_gt                4886
_reflns_number_total             7807
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic500012x_si_001.cif
_cod_data_source_block           JK575
_cod_depositor_comments
'Adding full bibliography for 4337916--4337924.cif.'
_cod_database_code               4337921
_shelx_estimated_absorpt_t_min   0.193
_shelx_estimated_absorpt_t_max   0.695
_shelxl_version_number           2013-4
_shelx_res_checksum              38172
_shelx_hkl_checksum              30997
_shelx_fab_checksum
'47172 CheckCif Responses No A or B Alerts detected'