2,2'-Iminobis(ethanaminium) (<i>p</i>-methyldihomooxacalix[4]arene)dioxouranium methanol disolvate monohydrate
Masci, Bernardo; Thuéry, Pierre; Acta Crystallographica Section E 63 (2007) m59–m61; doi:10.1107/S1600536806051580

data_2211790
_publ_section_title
;
 2,2'-Iminobis(ethanaminium)
 (<i>p</i>-methyldihomooxacalix[4]arene)dioxouranium methanol disolvate
 monohydrate
;
_journal_coeditor_code           DN2099
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m59
_journal_page_last               m61
_journal_paper_doi               10.1107/S1600536806051580
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac
'(C4 H15 N3) [U O2 (C33 H30 O5)], 2C H4 O, H2 O'
_chemical_formula_moiety
'C4 H15 N3 2+, C33 H30 O7 U 2-, 2(C H4 O), H2 O '
_chemical_formula_sum            'C39 H55 N3 O10 U'
_chemical_formula_weight         963.89
_chemical_name_systematic
;
diethylenetriamine(2+) (<i>p</i>-methyldihomooxacalix[4]arene)dioxouranium
methanol disolvate monohydrate
;
_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                 105.441(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9895(4)
_cell_length_b                   16.2079(3)
_cell_length_c                   21.2475(6)
_cell_measurement_reflns_used    131799
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.16
_cell_volume                     3979.88(19)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        HKL2000
_computing_molecular_graphics    'SHELXTL (Bruker, 1999)'
_computing_publication_material
'SHELXTL (Bruker, 1999) and 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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       'two \f and four \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  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0365
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            131799
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.137
_exptl_absorpt_correction_T_max  0.749
_exptl_absorpt_correction_T_min  0.528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light orange'
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.998
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         7565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0238
_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^)+(0.0321P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0553
_refine_ls_wR_factor_ref         0.0586
_reflns_number_gt                6173
_reflns_number_total             7565
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn2099.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2211790
_cod_database_fobs_code          2211790