Structural Variation within Homometallic Uranium(VI) Carboxyphosphonates: In Situ Ligand Synthesis, Directed Assembly, Metal-Ligand Coordination and Hydrogen Bonding
Karah E. Knope; Christopher L. Cahill; Inorganic Chemistry 47 (2008) 7660–7672; doi:10.1021/ic800683m

data_4305702
_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
;
Structural Variation within Homometallic Uranium(VI) Carboxyphosphonates:
In Situ Ligand Synthesis, Directed Assembly, Metal-Ligand Coordination
and Hydrogen Bonding
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7660
_journal_page_last               7672
_journal_paper_doi               10.1021/ic800683m
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C2 H2 O7 P U, H4 N, H2 O'
_chemical_formula_sum            'C2 H8 N O8 P U'
_chemical_formula_weight         443.09
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.5896(4)
_cell_length_b                   13.3487(6)
_cell_length_c                   13.4502(6)
_cell_measurement_reflns_used    14180
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      30.300
_cell_measurement_theta_min      3.023
_cell_volume                     1721.74(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker Apex CCD II'
_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  0.0587
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28628
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.30
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    19.059
_exptl_absorpt_correction_T_max  0.683
_exptl_absorpt_correction_T_min  0.264
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.893
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.918
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         2485
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.917
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0196
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0149P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0354
_refine_ls_wR_factor_ref         0.0374
_reflns_number_gt                1832
_reflns_number_total             2485
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800683m-file002_4.cif
_cod_data_source_block           pbca
_cod_database_code               4305702