Uranyl-Based Metallamacrocycles: Tri- and Tetranuclear Complexes with (2R,3R,4S,5S)-Tetrahydrofurantetracarboxylic Acid
Pierre Thuéry; Claude Villiers; Joël Jaud; Michel Ephritikhine; Bernardo Masci; Journal of the American Chemical Society 126 (2004) 6838–6839; doi:10.1021/ja0485964

data_4112626
_publ_contact_author_address
;
      CEA/Saclay, SCM (CNRS URA 331)
      B\^at. 125
      91191 Gif-sur-Yvette
      France
;
_publ_contact_author_email       thuery@drecam.cea.fr
_publ_contact_author_fax         '33 1 69 08 66 40'
_publ_contact_author_name        'P. Thu\'ery'
_publ_contact_author_phone       '33 01 69 08 63 29'
_publ_section_title
;
 Uranyl-Based Metallamacrocycles: Tri- and Tetranuclear Complexes with
 (2R,3R,4S,5S)-Tetrahydrofurantetracarboxylic Acid
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6838
_journal_page_last               6839
_journal_paper_doi               10.1021/ja0485964
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C66 H126 N6 O42 U3'
_chemical_formula_weight         2389.82
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   constr
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   19.139(3)
_cell_length_b                   19.139(3)
_cell_length_c                   18.5941(13)
_cell_measurement_reflns_used    20362
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      3.05
_cell_volume                     5898.5(14)
_computing_cell_refinement       'Eval-CCD (Duisenberg et al., 2003)'
_computing_data_collection       'Eval-CCD (Duisenberg et al., 2003)'
_computing_data_reduction        'Eval-CCD (Duisenberg et al., 2003)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material  'SHELXTL (Sheldrick, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.923
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       '\f 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  0.1075
_diffrn_reflns_av_sigmaI/netI    0.1113
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20362
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.05
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.178
_exptl_absorpt_correction_T_max  0.603
_exptl_absorpt_correction_T_min  0.256
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'program SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3573
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1258
_refine_ls_R_factor_gt           0.0644
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1009P)^2^+39.9750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1645
_refine_ls_wR_factor_ref         0.1998
_reflns_number_gt                2220
_reflns_number_total             3573
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0485964si20040311_042438.cif
_cod_data_source_block           1
_cod_original_cell_volume        5898.6(14)
_cod_database_code               4112626