Homometallic Uranium(VI) Phosphonoacetates Containing Interlayer Dipyridines
Karah E. Knope; Christopher L. Cahill; Inorganic Chemistry 48 (2009) 6845–6851; doi:10.1021/ic9007735

data_4302754
_publ_contact_author_address
;Department of Chemistry
George Washington University
725 21st Street, NW
Washington, DC 20052
;
_publ_contact_author_email       cahill@gwu.edu
_publ_contact_author_fax         202-994-5873
_publ_contact_author_name        'Christopher L. Cahill'
_publ_contact_author_phone       202-994-6959
_publ_section_title
;
Homometallic Uranium(VI) Phosphonoacetates Containing Interlayer Dipyridines
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6845
_journal_page_last               6851
_journal_paper_doi               10.1021/ic9007735
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C6 H9 O22 P3 U3, C10 H10 N2, 3(H2O)'
_chemical_formula_sum            'C16 H25 N2 O25 P3 U3'
_chemical_formula_weight         1452.38
_chemical_name_systematic
;
 ?
;
_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                 100.3130(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9801(4)
_cell_length_b                   25.5577(11)
_cell_length_c                   13.8436(6)
_cell_measurement_reflns_used    28445
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      30.22
_cell_measurement_theta_min      2.31
_cell_volume                     3125.9(2)
_computing_cell_refinement       ' APEX2 Software Suite (Bruker-AXS) '
_computing_data_collection       ' SMART V5.05 (Bruker-AXS) '
_computing_data_reduction        ' APEX2 Software Suite (Bruker-AXS) '
_computing_molecular_graphics    ' SHELXL-97 (Sheldrick, 1997) '
_computing_publication_material  ' WINGX (Farrugia, 1998) '
_computing_structure_refinement  ' SHELXL-97 (Sheldrick, 1997) '
_computing_structure_solution    ' SHELXS-97 (Sheldrick, 1990) '
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Bruker Apex II CCD'
_diffrn_measurement_method       'omega and phi 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  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            61358
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.43
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    15.763
_exptl_absorpt_correction_T_max  0.730
_exptl_absorpt_correction_T_min  0.474
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.086
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.693
_refine_diff_density_min         -1.759
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         8848
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0277
_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^)+(0.0110P)^2^+21.5226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0552
_refine_ls_wR_factor_ref         0.0585
_reflns_number_gt                7308
_reflns_number_total             8848
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9007735_si_002_2.cif
_cod_data_source_block           C16H25N2O25P3U3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4302754