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_4122185
_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         '2(C50 H71 N4 O5 U), 1.5(C6 H6)'
_chemical_formula_sum            'C109 H151 N8 O10 U2'
_chemical_formula_weight         2209.44
_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                 94.560(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3520(11)
_cell_length_b                   18.1081(9)
_cell_length_c                   37.4604(19)
_cell_measurement_reflns_used    431
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      12.00
_cell_measurement_theta_min      6.00
_cell_volume                     10380.9(11)
_computing_cell_refinement       'EVALCCD (Duisenberg, 2003)'
_computing_data_collection       'COLLECT (Bruker-Nonius, 2002)'
_computing_data_reduction        'EVALCCD (Duisenberg, 2003)'
_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 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
;
 \f- and \w-rotations with 0.60 \% and 72 sec per frame
;
_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  0.0496
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            175395
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    3.176
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4500
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.847
_refine_diff_density_min         -1.181
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1217
_refine_ls_number_reflns         24709
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0241P)^2^+8.1517P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0594
_reflns_number_gt                20806
_reflns_number_total             24709
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja504528n_si_002.cif
_cod_data_source_block           acs1115
_cod_depositor_comments
'Adding full bibliography for 4122183--4122197.cif.'
_cod_original_cell_volume        10380.7(10)
_cod_original_sg_symbol_Hall     -P2ybc
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4122185