Reductive Cleavage of Nitrite to Form Terminal Uranium Mono-Oxo Complexes
Andrew J. Lewis; Patrick J. Carroll; Eric J. Schelter; Journal of the American Chemical Society 135 (2013) 511–518; doi:10.1021/ja311057y

data_4119168
_publ_section_title
;
 Reductive Cleavage of Nitrite to Form Terminal Uranium Mono-Oxo Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              511
_journal_page_last               518
_journal_paper_doi               10.1021/ja311057y
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C52 H132 Cl2 F4 N6 O2 Si12 U2'
_chemical_formula_weight         1833.68
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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     direct
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.943(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.9455(10)
_cell_length_b                   19.6016(16)
_cell_length_c                   17.9892(15)
_cell_measurement_temperature    143(1)
_cell_volume                     4148.9(6)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      143(1)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            122940
_diffrn_reflns_theta_full        27.62
_diffrn_reflns_theta_max         27.62
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    4.182
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.825
_refine_diff_density_min         -1.490
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         9535
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0003P)^2^+46.0497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1158
_reflns_number_gt                7581
_reflns_number_total             9535
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja311057y_si_002_3.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               4119168