Inclusion of diprotonated [2.2.2]cryptand in the cavity of uranyl-complexed <i>p</i>-phenyltetrahomodioxacalix[4]arene
Masci, Bernardo; Levi Mortera, Stefano; Thuéry, Pierre; Acta Crystallographica Section C 61 (2005) m482–m484; doi:10.1107/S0108270105030581

data_2015119
_publ_section_title
;
 Inclusion of diprotonated [2.2.2]cryptand in the cavity of
 uranyl-complexed <i>p</i>-phenyltetrahomodioxacalix[4]arene
;
_journal_coeditor_code           DN1098
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m482
_journal_page_last               m484
_journal_paper_doi               10.1107/S0108270105030581
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac
'(C18 H38 N2 O6) [U (C54 H40 O6) O2], 3C2 H6 O S'
_chemical_formula_moiety         'C18 H38 N2 O6 2+, C54 H40 O8 U 2-, 3C2 H6 O S'
_chemical_formula_sum            'C78 H96 N2 O17 S3 U'
_chemical_formula_weight         1667.78
_chemical_name_systematic
;
4,7,13,16,21,24-hexaoxa-1,10-diazoniabicyclo[8.8.8]hexacosane
[7,13,21,27-tetraphenyl-3,17-
dioxapentacyclo[23.3.1.1^5,9^.1^11,15^.1^9,23^]ditriaconta-
1(29),5,7,9(30),11(31),12,14,19(32),20,22,25,27-dodecaene-29,30,31,32-
tetraolato]dioxouranium dimethylsulfoxide trisolvate
;
_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                 106.169(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8955(5)
_cell_length_b                   20.3681(10)
_cell_length_c                   24.9276(11)
_cell_measurement_reflns_used    190557
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.91
_cell_volume                     7263.7(5)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1999)'
_computing_publication_material  'SHELXTL (Bruker, 1999); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector diffractometer'
_diffrn_measurement_method       'two \f and three \w scans with 2\% steps'
_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  0.0822
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            190557
_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
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.392
_exptl_absorpt_correction_T_max  0.787
_exptl_absorpt_correction_T_min  0.603
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   '[DELABS in PLATON (Spek, 2003)]'
_exptl_crystal_colour            'translucent light orange'
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3416
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.536
_refine_diff_density_min         -1.257
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     922
_refine_ls_number_reflns         13724
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0524
_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^)+(0.0659P)^2^+43.6206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1348
_refine_ls_wR_factor_ref         0.1458
_reflns_number_gt                10606
_reflns_number_total             13724
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn1098.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2015119
_cod_database_fobs_code          2015119