Bis{<i>N</i>-[bis(pyrrolidin-1-yl)phosphoryl]-2,2,2-trichloroacetamide}dinitratodioxidouranium(VI)
Znovjyak, Kateryna O.; Ovchynnikov, Vladimir A.; Moroz, Olesia V.; Shishkina, Svitlana V.; Amirkhanov, Vladimir M.; Acta Crystallographica Section E 66 (2010) m322–; doi:10.1107/S1600536810006422

data_2225222
_publ_section_title
Bis{<i>N</i>-[bis(pyrrolidin-1-yl)phosphoryl]-2,2,2-trichloroacetamide}dinitratodioxidouranium(VI)
_journal_coeditor_code           DN2539
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m322
_journal_paper_doi               10.1107/S1600536810006422
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[U (N O3)2 O2 (C10 H17 Cl3 N3 O2 P)2]'
_chemical_formula_moiety         'C20 H34 Cl6 N8 O12 P2 U'
_chemical_formula_sum            'C20 H34 Cl6 N8 O12 P2 U'
_chemical_formula_weight         1091.22
_chemical_name_systematic
;
Bis{<i>N</i>-[bis(pyrrolidin-1-yl)phosphoryl]-2,2,2-
trichloroacetamide}dinitratodioxidouranium(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                71.905(6)
_cell_angle_beta                 84.391(5)
_cell_angle_gamma                71.475(6)
_cell_formula_units_Z            1
_cell_length_a                   9.8292(7)
_cell_length_b                   10.3436(8)
_cell_length_c                   10.4475(6)
_cell_measurement_reflns_used    35271
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      40.84
_cell_measurement_theta_min      3.00
_cell_volume                     957.34(12)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2006)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2006)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2006)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Burnett & Johnson, 1996; Farrugia, 1997)
;
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1827
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur3 diffractometer'
_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  0.0896
_diffrn_reflns_av_sigmaI/netI    0.0493
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22849
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    4.804
_exptl_absorpt_correction_T_max  0.4467
_exptl_absorpt_correction_T_min  0.2496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2006)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.893
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             530
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.930
_refine_diff_density_min         -1.681
_refine_ls_extinction_coef       0.0164(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         5523
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0645P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0847
_reflns_number_gt                5486
_reflns_number_total             5523
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            dn2539.cif
_cod_data_source_block           I
_cod_original_cell_volume        957.34(11)
_cod_database_code               2225222
_cod_database_fobs_code          2225222