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_4122192
_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         'C90 H132 N6 O8 U2, C18 H36 K N2 O6, 3(C6 H6)'
_chemical_formula_sum            'C126 H186 K N8 O14 U2'
_chemical_formula_weight         2551.99
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.896(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.189(2)
_cell_length_b                   25.230(4)
_cell_length_c                   36.900(6)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.69
_cell_measurement_theta_min      2.61
_cell_volume                     12250(3)
_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      150(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar focussing montel optics'
_diffrn_radiation_source         'ImuS micro-focus tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_sigmaI/netI    0.0750
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            101231
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    2.737
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2008'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5252
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.132
_refine_diff_density_min         -1.606
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1539
_refine_ls_number_reflns         26919
_refine_ls_number_restraints     444
_refine_ls_restrained_S_all      1.208
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+3.2059P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.0958
_reflns_number_gt                18263
_reflns_number_total             26919
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja504528n_si_002.cif
_cod_data_source_block           acs1224
_cod_depositor_comments
'Adding full bibliography for 4122183--4122197.cif.'
_cod_original_cell_volume        12251(3)
_cod_original_sg_symbol_Hall     -P2ybc
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4122192