Bis(1,3-diphenylpropane-1,3-dionato-κ^2^<i>O,O</i>')dioxo(triphenylphosphine oxide-κ<i>O</i>)uranium(VI)
M. Alagar; K.Rajagopal; R.V. Krishnakumar; M. Subha Nandhini; S. Kannan; S.Natarajan; Acta Crystallographica Section E 59 (2003) m524–m526; doi:10.1107/S1600536803012923

data_2202467
_publ_section_title
;Bis(1,3-diphenylpropane-1,3-dionato-\k^2^<i>O,O</i>')dioxo(triphenylphosphine
 oxide-\k<i>O</i>)uranium(VI)
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m524
_journal_page_last               m526
_journal_paper_doi               10.1107/S1600536803012923
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[U O2 (C15 H11 O2)2 (C18 H15 O1 P1)]'
_chemical_formula_moiety         'C48 H37 O7 P U'
_chemical_formula_sum            'C48 H37 O7 P U'
_chemical_formula_weight         994.78
_chemical_name_systematic
;
Bis(1,3-diphenylpropane-1,3-dionato-\k^2^O,O')dioxo(triphenylphosphine
oxide-\kO)uranium(VI)
;
_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                 103.170(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.345(2)
_cell_length_b                   11.022(4)
_cell_length_c                   20.924(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     4119.5(18)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'CAD-4 Software'
_computing_molecular_graphics    'PLATON (Spek, 1999)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w-2\q
_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  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0434
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7464
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_time  60min
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    4.031
_exptl_absorpt_correction_T_max  0.597
_exptl_absorpt_correction_T_min  0.325
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.916
_refine_ls_extinction_coef       0.00049(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.288
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         7221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.288
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0316P)^2^+1.9225P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0842
_reflns_number_gt                5259
_reflns_number_total             7221
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci6234.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2202467
_cod_database_fobs_code          2202467