The chloroform-solvated uranyl complex of <i>p</i>-<i>tert</i>-butylhexahomotrioxacalix[3]arene with the chiral counter-ion (<i>S</i>)-(–)-<i>N</i>,α-dimethylbenzylammonium
Masci, Bernardo; Thuéry, Pierre; Acta Crystallographica Section E 61 (2005) m2278–m2280; doi:10.1107/S1600536805031867

data_2207212
_publ_section_title
;
 The chloroform-solvated uranyl complex of
 <i>p</i>-<i>tert</i>-butylhexahomotrioxacalix[3]arene with the chiral
 counter-ion (<i>S</i>)-(--)-<i>N</i>,\a-dimethylbenzylammonium
;
_journal_coeditor_code           DN6262
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2278
_journal_page_last               m2280
_journal_paper_doi               10.1107/S1600536805031867
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '(C9 H14 N) [U O2 (C36 H45 O6)], C H Cl3'
_chemical_formula_moiety         'C9 H14 N +, C36 H45 O8 U -, C H Cl3'
_chemical_formula_sum            'C46 H60 Cl3 N O8 U'
_chemical_formula_weight         1099.33
_chemical_name_systematic
;(S)-(-)-N,\a-dimethylbenzylammonium
dioxo[7,15,23-tri-tert-butyl-3,11,19-trioxatetracyclo[19.3.1.1^5,9^.1^13,17^]
heptacosa-1(25),5,7,9(27),13,15,17(26),21,23-nonaene-25,26,27-triolato]uranium
trichloromethane
 solvate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6605(3)
_cell_length_b                   21.2825(10)
_cell_length_c                   22.8491(11)
_cell_measurement_reflns_used    82013
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.62
_cell_volume                     4697.8(3)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        HKL2000
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       'two \f and one \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  0.0619
_diffrn_reflns_av_sigmaI/netI    0.0570
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            82013
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.62
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.677
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_correction_T_min  0.527
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   '(DELABS in PLATON; Spek, 2003)'
_exptl_crystal_colour            'translucent dark orange'
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2200
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.827
_refine_ls_abs_structure_details 'Flack  (1983), 3779 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.010(5)
_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     543
_refine_ls_number_reflns         8750
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0114P)^2^+4.555P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0652
_reflns_number_gt                8052
_reflns_number_total             8750
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn6262.cif
_cod_data_source_block           I
_cod_database_code               2207212
_cod_database_fobs_code          2207212