New polynuclear U(IV)-U(V) complexes from U(IV) mediated uranyl(V) disproportionation.
Mougel, Victor; Pécaut, Jacques; Mazzanti, Marinella; Chemical communications (Cambridge, England) 48 (2012) 868–870; doi:10.1039/c1cc16646h

data_7112555
_publ_section_title
;
 New polynuclear U(IV)-U(V) complexes from U(IV) mediated uranyl(V)
 disproportionation.
;
_journal_issue                   6
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              868
_journal_page_last               870
_journal_paper_doi               10.1039/c1cc16646h
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C38 H42 N6 O8 U2'
_chemical_formula_weight         1186.84
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_symmetry_space_group_name_Hall  '-P 2ybc'
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_cell_angle_beta                 105.356(3)
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_cell_formula_units_Z            4
_cell_length_a                   16.3093(7)
_cell_length_b                   10.8301(2)
_cell_length_c                   22.1561(6)
_cell_measurement_reflns_used    6433
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.3061
_cell_measurement_theta_min      3.3054
_cell_volume                     3773.7(2)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
1 omega -26.00 75.00 1.0000 50.0000
omega____ theta____ kappa____ phi______ frames
- 25.4051 0.0000 -120.0000 101

2 omega -5.00 96.00 1.0000 50.0000
omega____ theta____ kappa____ phi______ frames
- 25.4051 77.0000 -150.0000 101

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
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_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  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0637
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            18306
_diffrn_reflns_theta_full        30.45
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         3.36
_exptl_absorpt_coefficient_mu    8.632
_exptl_absorpt_correction_T_max  0.5873
_exptl_absorpt_correction_T_min  0.2571
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.089
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bloc
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.747
_refine_diff_density_min         -1.197
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         11399
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0192P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0684
_reflns_number_gt                8853
_reflns_number_total             11399
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc16646h.txt
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7112555