Formation of Lanthanide and Actinide Oxonium Ion Complexes with Crown Ethers from a Liquid Clathrate Medium
Hany Hassaballa; Jonathan W. Steed; Peter C. Junk; Mark R. J. Elsegood; Inorganic Chemistry 37 (1998) 4666–4671; doi:10.1021/ic9802597

data_4322999
_publ_section_title
;
 Formation of Lanthanide and Actinide Oxonium Ion Complexes with Crown
 Ethers from a Liquid Clathrate Medium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4666
_journal_page_last               4671
_journal_paper_doi               10.1021/ic9802597
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C10 H26 Cl2 O10 U'
_chemical_formula_weight         615.24
_chemical_name_common            'compound 7'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           145
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 32'
_symmetry_space_group_name_H-M   'P 32'
_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                120.00
_cell_formula_units_Z            48
_cell_length_a                   35.3500(2)
_cell_length_b                   35.3500(2)
_cell_length_c                   21.3755(2)
_cell_measurement_temperature    173(2)
_cell_volume                     23132.7(3)
_computing_cell_refinement       DENZO-SMN
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    RES2INS
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  KappaCCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0970
_diffrn_reflns_av_sigmaI/netI    0.0557
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            153662
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    8.738
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.120
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polygon
_exptl_crystal_F_000             14016
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.950
_refine_diff_density_min         -4.771
_refine_diff_density_rms         0.256
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.041(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     3305
_refine_ls_number_reflns         51913
_refine_ls_number_restraints     3888
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0722
_refine_ls_shift/su_max          0.072
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0242P)^2^+966.2700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1500
_refine_ls_wR_factor_ref         0.1575
_reflns_number_gt                45587
_reflns_number_total             51913
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9802597_5.cif
_cod_data_source_block           15c5ult
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0242P)^2^+966.2700P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0242P)^2^+966.2700P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4322999