Synthesis and crystal structure of 1:2 mixed uranyl/alkali metal ions (Li+, Na+, K+, Cs+) complexes of p-tert-butyltetrahomodioxacalix[4]arene
Pierre Thuéry; Bernardo Masci; Dalton Trans.  (2003) 2411–2417; doi:10.1039/b302233a

data_7012879
_publ_section_title
;
 Synthesis and crystal structure of 1:2 mixed uranyl/alkali metal ions
 (Li+, Na+, K+, Cs+) complexes of
 p-tert-butyltetrahomodioxacalix[4]arene
;
_journal_issue                   12
_journal_name_full               'Dalton Trans.'
_journal_page_first              2411
_journal_page_last               2417
_journal_paper_doi               10.1039/b302233a
_journal_year                    2003
_chemical_formula_sum            'C49 H82 Li2 O18 U'
_chemical_formula_weight         1211.06
_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                 98.597(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5382(11)
_cell_length_b                   19.656(2)
_cell_length_c                   23.1000(19)
_cell_measurement_reflns_used    32084
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.71
_cell_volume                     5629.0(9)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa-CCD software (Nonius B.V., 1998)'
_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, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0727
_diffrn_reflns_av_sigmaI/netI    0.1148
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            32084
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.71
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    2.949
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.347
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2000)'
_exptl_crystal_colour            'translucent light orange'
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_meas      ?
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.064
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     646
_refine_ls_number_reflns         10526
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1194
_refine_ls_R_factor_gt           0.0608
_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^)+(0.0686P)^2^+2.3200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1629
_reflns_number_gt                6449
_reflns_number_total             10526
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b302233a.txt
_cod_data_source_block           1
_cod_original_cell_volume        5629.2(9)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7012879