Crystal structure of dioxidobis(pentane-2,4-dionato-κ^2^<i>O</i>,<i>O</i>')[1-phenyl-3-(pyridin-4-yl)propane-κ<i>N</i>]uranium(VI)
Kawasaki, Takeshi; Kitazawa, Takafumi; Acta Crystallographica Section E 71 (2015) 42–44; doi:10.1107/S2056989014026607

data_2240305
_publ_section_title
;
 Crystal structure of
 dioxidobis(pentane-2,4-dionato-\k^2^<i>O</i>,<i>O</i>')[1-phenyl-3-(pyridin-4-yl)propane-\k<i>N</i>]uranium(VI)
;
_journal_coeditor_code           CQ2012
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              42
_journal_page_last               44
_journal_paper_doi               10.1107/S2056989014026607
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[U (C5 H7 O2)2 O2 (C14 H15 N)]'
_chemical_formula_moiety         'C24 H29 N O6 U'
_chemical_formula_sum            'C24 H29 N O6 U'
_chemical_formula_weight         665.51
_chemical_name_systematic
Dioxidobis(pentane-2,4-dionato-\k^2^<i>O</i>,<i>O</i>')[1-phenyl-3-(pyridin-4-yl)propane-\k<i>N</i>]uranium(VI)
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.67(3)
_cell_angle_beta                 98.50(3)
_cell_angle_gamma                100.81(3)
_cell_formula_units_Z            2
_cell_length_a                   8.2100(16)
_cell_length_b                   11.530(2)
_cell_length_c                   14.516(3)
_cell_measurement_reflns_used    4311
_cell_measurement_temperature    297
_cell_measurement_theta_max      28.5
_cell_measurement_theta_min      2.59
_cell_volume                     1246.4(5)
_computing_cell_refinement
;
SAINT (Bruker, 2007) and XSCANS (Bruker, 2007)
;
_computing_data_collection
;
APEX2 (Bruker, 2007) and XSCANS (Bruker, 2007)
;
_computing_data_reduction
;
APEX2 (Bruker, 2007) and SAINT (Bruker, 2007)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and ORTEP-3 for Windows (Farrugia,
2012)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      297
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_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  0.0149
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9353
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.89
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    6.548
_exptl_absorpt_correction_T_max  0.2808
_exptl_absorpt_correction_T_min  0.1488
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(XPREP; Bruker, 2007)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.883
_refine_diff_density_min         -0.643
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         6948
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0539
_refine_ls_wR_factor_ref         0.0560
_reflns_number_gt                6026
_reflns_number_total             6948
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cq2012sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        1246.4(4)
_cod_database_code               2240305
_cod_database_fobs_code          2240305