Molecular and Electronic Structure of Dinuclear Uranium Bis-μ-Oxo Complexes with Diamond Core Structural Motifs.
Schmidt, Anna-Corina; Heinemann, Frank W.; Lukens, Jr, Wayne W; Meyer, Karsten; Journal of the American Chemical Society 136 (2014) 11980–; doi:10.1021/ja504528n

data_4122193
_publ_section_title
;
 Molecular and Electronic Structure of Dinuclear Uranium Bis-\m-Oxo
 Complexes with Diamond Core Structural Motifs.
;
_journal_issue                   34
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11980
_journal_paper_doi               10.1021/ja504528n
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C46 H66 F3 N3 O7 S U, 2(C6 H6)'
_chemical_formula_sum            'C58 H78 F3 N3 O7 S U'
_chemical_formula_weight         1256.32
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.757(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.153(3)
_cell_length_b                   15.4977(11)
_cell_length_c                   25.339(2)
_cell_measurement_reflns_used    9658
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.84
_cell_measurement_theta_min      2.47
_cell_volume                     11371.9(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_refinement  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Bruker Smart APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            114326
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.03
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    2.954
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2008'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5104
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.699
_refine_diff_density_min         -1.512
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         14411
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+3.0958P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0728
_reflns_number_gt                11365
_reflns_number_total             14411
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja504528n_si_002.cif
_cod_data_source_block           acs1302
_cod_depositor_comments
'Adding full bibliography for 4122183--4122197.cif.'
_cod_original_cell_volume        11372.0(17)
_cod_original_sg_symbol_Hall     -C2yc
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4122193