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_4305699
_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         'C9 H13 O21 P3 U3, 2 H2O, 2 NH4'
_chemical_formula_sum            'C9 H25 N2 O23 P3 U3'
_chemical_formula_weight         1336.31
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 104.2950(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.7542(6)
_cell_length_b                   17.8712(12)
_cell_length_c                   9.0548(6)
_cell_measurement_reflns_used    25037
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      30.41
_cell_measurement_theta_min      2.28
_cell_volume                     1372.74(16)
_computing_cell_refinement       ' SAINT (Bruker-AXS) '
_computing_data_collection       ' SMART V5.05 (Bruker-AXS) '
_computing_data_reduction        ' SAINT (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 0.991
_diffrn_measured_fraction_theta_max 0.931
_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  0.0656
_diffrn_reflns_av_sigmaI/netI    0.0738
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            25037
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.41
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    17.926
_exptl_absorpt_correction_T_max  0.699
_exptl_absorpt_correction_T_min  0.657
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.582
_refine_diff_density_min         -1.405
_refine_diff_density_rms         0.224
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.828
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3996
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.828
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0104P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0405
_refine_ls_wR_factor_ref         0.0433
_reflns_number_gt                2892
_reflns_number_total             3996
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800683m-file002_1.cif
_cod_data_source_block           p21onm
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'EMPIRICAL' changed to 'empirical'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               4305699