Dihydro[2.2.2]cryptand di-μ-hydroxo-bis[bis(nitrato-κ^2^<i>O</i>,<i>O</i>')dioxouranium(VI)] monohydrate
Thuéry, Pierre; Masci, Bernardo; Acta Crystallographica Section C 58 (2002) m556–m558; doi:10.1107/S0108270102018759

data_2013053
_publ_section_title
;
 Dihydro[2.2.2]cryptand
 di-\m-hydroxo-bis[bis(nitrato-\k^2^<i>O</i>,<i>O</i>')dioxouranium(VI)]
 monohydrate
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m556
_journal_page_last               m558
_journal_paper_doi               10.1107/S0108270102018759
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '(C18 H38 N2 O6) [U2 O4 (N O3)4 (O H)2] , H2 O'
_chemical_formula_moiety         'C18 H38 N2 O6 2+ , H2 N4 O18 U2 2- , H2 O'
_chemical_formula_sum            'C18 H42 N6 O25 U2'
_chemical_formula_weight         1218.64
_chemical_name_systematic
;
Dihydro[2.2.2]cryptand (2+)
di-\m-hydroxo-bis[bis(nitrato-\k^2^O,O')dioxouranium(VI)]
monohydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                86.528(3)
_cell_angle_beta                 82.042(3)
_cell_angle_gamma                74.826(3)
_cell_formula_units_Z            2
_cell_length_a                   9.0595(5)
_cell_length_b                   9.8517(5)
_cell_length_c                   20.8019(12)
_cell_measurement_reflns_used    12164
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.79
_cell_volume                     1774.04(17)
_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 PARST97 (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.924
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       \f
_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  0.039
_diffrn_reflns_av_sigmaI/netI    0.061
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            12164
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.79
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    9.218
_exptl_absorpt_correction_T_max  0.398
_exptl_absorpt_correction_T_min  0.201
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(DELABS in PLATON; Spek, 2000)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    2.281
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.92
_refine_diff_density_min         -0.90
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         6199
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.041
_refine_ls_R_factor_gt           0.028
_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^)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.063
_refine_ls_wR_factor_ref         0.068
_reflns_number_gt                5014
_reflns_number_total             6199
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sq1000.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-1
_cod_database_code               2013053
_cod_database_fobs_code          2013053