New insights into the acid mediated disproportionation of pentavalent uranyl.
Victor Mougel; Biplab Biswas; Jacques Pecaut; Marinella Mazzanti; Chem.Commun. 46 (2010) 8648–; doi:10.1039/c0cc03443f

data_7105692
_publ_section_title
;
 New insights into the acid mediated disproportionation of pentavalent
 uranyl.
;
_journal_name_full               Chem.Commun.
_journal_page_first              8648
_journal_paper_doi               10.1039/c0cc03443f
_journal_volume                  46
_journal_year                    2010
_chemical_formula_sum            'C113 H95 N7 O32 U6'
_chemical_formula_weight         3491.14
_chemical_name_systematic
;
?
;
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.4352(4)
_cell_length_b                   16.3250(2)
_cell_length_c                   28.7642(4)
_cell_measurement_reflns_used    23894
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.3654
_cell_measurement_theta_min      3.3151
_cell_volume                     12882.9(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
1 omega 50.00 75.50 0.7500 30.0000
omega____ theta____ kappa____ phi______ frames
- 25.2489 179.0000 30.0000 34

2 omega 33.00 90.75 0.7500 30.0000
omega____ theta____ kappa____ phi______ frames
- 25.2489 -139.0000 140.0000 77

3 omega 34.00 89.50 0.7500 30.0000
omega____ theta____ kappa____ phi______ frames
- 25.2489 -139.0000 -20.0000 74

4 omega 49.00 74.50 0.7500 30.0000
omega____ theta____ kappa____ phi______ frames
- 25.2489 179.0000 -180.0000 34

5 omega -90.00 -32.25 0.7500 30.0000
omega____ theta____ kappa____ phi______ frames
- -27.1239 179.0000 -90.0000 77

6 omega -49.00 18.50 0.7500 30.0000
omega____ theta____ kappa____ phi______ frames
- -27.1239 37.0000 -120.0000 90

7 omega -54.00 -25.50 0.7500 30.0000
omega____ theta____ kappa____ phi______ frames
- -27.1239 77.0000 -180.0000 38

8 omega -85.00 45.50 0.7500 30.0000
omega____ theta____ kappa____ phi______ frames
- -27.1239 0.0000 -180.0000 174

9 omega -97.00 -46.00 0.7500 30.0000
omega____ theta____ kappa____ phi______ frames
- -27.1239 -77.0000 120.0000 68

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\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  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            66545
_diffrn_reflns_theta_full        28.20
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.32
_exptl_absorpt_coefficient_mu    7.586
_exptl_absorpt_correction_T_max  0.4810
_exptl_absorpt_correction_T_min  0.1992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.800
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'monoclinic prism'
_exptl_crystal_F_000             6520
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         5.447
_refine_diff_density_min         -5.634
_refine_diff_density_rms         0.403
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         8304
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0865
_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^)+(0.1353P)^2^+484.7964P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2655
_refine_ls_wR_factor_ref         0.2725
_reflns_number_gt                5833
_reflns_number_total             8304
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CC03443F.TXT
_cod_data_source_block           vm197_3
_cod_database_code               7105692