Pentavalent uranyl stabilized by a dianionic bulky tetradentate ligand.
Horeglad, Pawel; Nocton, Grégory; Filinchuk, Yaroslav; Pécaut, Jacques; Mazzanti, Marinella; Chemical communications (Cambridge, England) 34 (2009) 1843–1845; doi:10.1039/b821398d

data_7104305
_publ_section_title
;
 Pentavalent uranyl stabilized by a dianionic bulky tetradentate
 ligand.
;
_journal_issue                   14
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1843
_journal_page_last               1845
_journal_paper_doi               10.1039/b821398d
_journal_volume                  34
_journal_year                    2009
_chemical_formula_sum            'C40.5 H62.5 N3 O4 U'
_chemical_formula_weight         893.47
_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                 101.116(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.6726(6)
_cell_length_b                   20.0780(6)
_cell_length_c                   11.4096(3)
_cell_measurement_reflns_used    6467
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.9707
_cell_measurement_theta_min      3.0488
_cell_volume                     4422.1(2)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_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 0.821
_diffrn_measured_fraction_theta_max 0.821
_diffrn_measurement_details
;
1 omega -5.00 47.00 1.0000 180.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 17.1550 -77.0000 240.0000 0.0000 0.0000 52

2 omega 3.00 37.00 1.0000 180.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 17.1550 -135.0000 231.0000 0.0000 0.0000 34

3 omega -42.00 7.00 1.0000 180.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -18.7175 45.0000 60.0000 0.0000 0.0000 49

4 omega 3.00 43.00 1.0000 180.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -18.7175 -134.0000 62.0000 0.0000 0.0000 40

5 omega -90.00 3.00 1.0000 180.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -18.7175 -45.0000 90.0000 0.0000 0.0000 93

6 omega 4.00 46.00 1.0000 180.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -18.7175 0.0000 270.0000 0.0000 0.0000 42

;
_diffrn_measurement_device_type  XCalibur-S
_diffrn_measurement_method       omega-scan
_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  0.0464
_diffrn_reflns_av_sigmaI/netI    0.1361
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            25664
_diffrn_reflns_theta_full        28.95
_diffrn_reflns_theta_max         28.95
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    3.708
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_correction_T_min  0.860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSPACK (Oxford Diffraction, 2006)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1802
_exptl_crystal_size_max          0.3757
_exptl_crystal_size_mid          0.0338
_exptl_crystal_size_min          0.0171
_refine_diff_density_max         1.907
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.808
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         9620
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.809
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0280P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0745
_reflns_number_gt                5228
_reflns_number_total             9620
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b821398d.txt
_cod_data_source_block           3
_cod_original_formula_sum        'C40.50 H62.50 N3 O4 U'
_cod_database_code               7104305