Uranyl ions as supramolecular linkers in a bis(hexahomotrioxacalix[6]arene) hexa-uranate complex
Thuéry, Pierre; Nierlich, Martine; Vicens, Jacques; Masci, Bernardo; Journal of the Chemical Society, Dalton Transactions  (2001) 3410–; doi:10.1039/b109451n

data_7011246
_publ_section_title
;
 Uranyl ions as supramolecular linkers in a
 bis(hexahomotrioxacalix[6]arene) hexa-uranate complex
;
_journal_issue                   23
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3410
_journal_paper_doi               10.1039/b109451n
_journal_year                    2001
_chemical_formula_sum            'C99 H155.5 Cl7.5 N9 O24.5 U3'
_chemical_formula_weight         2843.79
_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                 103.992(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.301(2)
_cell_length_b                   30.908(2)
_cell_length_c                   19.427(2)
_cell_measurement_reflns_used    70266
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      5.10
_cell_volume                     11828.1(19)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa-CCD software (Nonius B.V., 1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_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, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_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  0.0988
_diffrn_reflns_av_sigmaI/netI    0.0935
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            70266
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         5.10
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.335
_exptl_absorpt_correction_T_max  0.648
_exptl_absorpt_correction_T_min  0.285
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2000)'
_exptl_crystal_colour            'translucent dark orange'
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_meas      ?
_exptl_crystal_description       platelet
_exptl_crystal_F_000             5648
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.355
_refine_diff_density_min         -1.119
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1332
_refine_ls_number_reflns         21363
_refine_ls_number_restraints     197
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.2343
_refine_ls_R_factor_gt           0.0817
_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^)+(0.0417P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1271
_refine_ls_wR_factor_ref         0.1752
_reflns_number_gt                8228
_reflns_number_total             21363
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b109451n.txt
_cod_data_source_block           1
_cod_original_cell_volume        11828(2)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C99 H155.50 Cl7.50 N9 O24.50 U3'
_cod_database_code               7011246