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_7012882
_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            'C50 H71.5 Cl1.5 Cs2 O12 U'
_chemical_formula_weight         1421.60
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 121.606(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   36.118(2)
_cell_length_b                   16.2137(9)
_cell_length_c                   23.4909(14)
_cell_measurement_reflns_used    33693
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.91
_cell_volume                     11716.0(13)
_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 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.1125
_diffrn_reflns_av_sigmaI/netI    0.1144
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            33693
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.91
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    4.117
_exptl_absorpt_correction_T_max  0.814
_exptl_absorpt_correction_T_min  0.188
_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    1.612
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             5560
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.933
_refine_diff_density_min         -1.177
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         10927
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1306
_refine_ls_R_factor_gt           0.0695
_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^)+(0.0580P)^2^+113.7934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1443
_refine_ls_wR_factor_ref         0.1710
_reflns_number_gt                6583
_reflns_number_total             10927
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b302233a.txt
_cod_data_source_block           4
_cod_original_cell_volume        11716.1(12)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C50 H71.50 Cl1.50 Cs2 O12 U'
_cod_database_code               7012882