Uranyl ion complexation by medium and large homooxacalixarenes: from mono- to poly-uranate complexes
Thuéry, Pierre; Nierlich, Martine; Vicens, Jacques; Masci, Bernardo; Journal of the Chemical Society, Dalton Transactions  (2001) 867–; doi:10.1039/b009364p

data_7010463
_publ_section_title
;
 Uranyl ion complexation by medium and large homooxacalixarenes: from
 mono- to poly-uranate complexes
;
_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              867
_journal_paper_doi               10.1039/b009364p
_journal_year                    2001
_chemical_formula_sum            'C86 H125 N5 O10 U'
_chemical_formula_weight         1626.94
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.590(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.5673(5)
_cell_length_b                   29.5268(16)
_cell_length_c                   33.0321(18)
_cell_measurement_reflns_used    101135
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.60
_cell_volume                     16894.5(14)
_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      110(2)
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full 0.924
_diffrn_measured_fraction_theta_max 0.924
_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  0.139
_diffrn_reflns_av_sigmaI/netI    0.131
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            101135
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.60
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.979
_exptl_absorpt_correction_T_max  0.669
_exptl_absorpt_correction_T_min  0.631
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
program MULABS from PLATON (Spek, 1997)
;
_exptl_crystal_colour            'translucent dark orange'
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle-like
_exptl_crystal_F_000             6784
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.051
_refine_diff_density_min         -1.231
_refine_diff_density_rms         0.137
_refine_ls_extinction_coef       0.00023(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1460
_refine_ls_number_reflns         29617
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.1439
_refine_ls_R_factor_gt           0.0672
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+18.0262P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1277
_refine_ls_wR_factor_ref         0.1559
_reflns_number_gt                16819
_reflns_number_total             29617
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b009364p.txt
_cod_data_source_block           5
_cod_original_cell_volume        16895(2)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7010463