A uranyl ion complex of <i>N</i>-methyl-<i>p</i>-<i>tert</i>-butyldihomoammoniocalix[4]arene with diaquadipyridinelithium as counter-ion
Thuéry, Pierre; Takemura, Hiroyuki; Acta Crystallographica Section C 59 (2003) m384–m386; doi:10.1107/S0108270103015786

data_2013667
_publ_section_title
;
 A uranyl ion complex of
 <i>N</i>-methyl-<i>p</i>-<i>tert</i>-butyldihomoammoniocalix[4]arene
 with diaquadipyridinelithium as counter-ion
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m384
_journal_page_last               m386
_journal_paper_doi               10.1107/S0108270103015786
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac
'[Li (C5 H5 N)2 (H2 O)2] [U O2 (C46 H58 N O4)], 3C5 H5 N, H2 O'
_chemical_formula_moiety
'C10 H14 Li N2 O2 1+, C46 H58 N O6 U 1-, 3C5 H5 N, H2 O'
_chemical_formula_sum            'C71 H89 Li N6 O9 U'
_chemical_formula_weight         1415.45
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 96.321(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.8644(16)
_cell_length_b                   16.6147(13)
_cell_length_c                   19.7150(14)
_cell_measurement_reflns_used    45959
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.66
_cell_volume                     6792.8(9)
_computing_cell_refinement       'DENZO--SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_data_reduction        DENZO--SMN
_computing_molecular_graphics    'SHELXTL (Bruker, 1999)'
_computing_publication_material  'SHELXTL 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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0962
_diffrn_reflns_av_sigmaI/netI    0.1225
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45959
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.66
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    2.449
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_correction_T_min  0.698
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   '(DELABS in PLATON; Spek, 2003)'
_exptl_crystal_colour            'translucent dark orange'
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_meas      ?
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2896
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.821
_refine_diff_density_min         -1.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     806
_refine_ls_number_reflns         12756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1198
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0088P)^2^+25.0468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1260
_reflns_number_gt                7934
_reflns_number_total             12756
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob1134.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2013667
_cod_database_fobs_code          2013667