Non-Centrosymmetric Tetrameric Assemblies of Tetramethylammonium Halides with Uranyl Salophen Complexes in the Solid State
Massimo Cametti; Laura Ilander; Arto Valkonen; Martin Nieger; Maija Nissinen; Elisa Nauha; Kari Rissanen; Inorganic Chemistry 49 (2010) 11473–11484; doi:10.1021/ic101547r

data_4317311
_publ_section_title
;
 Non-Centrosymmetric Tetrameric Assemblies of Tetramethylammonium Halides
 with Uranyl Salophen Complexes in the Solid State
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11473
_journal_page_last               11484
_journal_paper_doi               10.1021/ic101547r
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety
;
'3(C36 H30 Cl N2 O8 U), 4(C4 H12 N), 3(C H Cl3), Cl'
;
_chemical_formula_sum            'C127 H141 Cl13 N10 O24 U3'
_chemical_formula_weight         3366.44
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           220
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'I -4bd 2c 3'
_symmetry_space_group_name_H-M   'I -4 3 d'
_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            16
_cell_length_a                   37.759(4)
_cell_length_b                   37.759(4)
_cell_length_c                   37.759(4)
_cell_measurement_reflns_used    8413
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.71
_cell_measurement_theta_min      2.95
_cell_volume                     53835(10)
_computing_cell_refinement
;
'HKL Scalepack (Otwinowski & Minor 1997)'
;
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
'HKL Denzo and Scalepack (Otwinowski & Minor 19'
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'nonius KappaCCD'
_diffrn_measurement_method       'psi and omega scan'
_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  0.1210
_diffrn_reflns_av_sigmaI/netI    0.0842
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            37429
_diffrn_reflns_theta_full        25.71
_diffrn_reflns_theta_max         25.71
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    3.930
_exptl_absorpt_correction_T_max  0.8277
_exptl_absorpt_correction_T_min  0.3024
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
'R. H. Blessing, Acta Crystallogr.A 1995, 51, 33'  
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             26592
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.974
_refine_diff_density_min         -1.032
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.007(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         8413
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+459.3228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1177
_reflns_number_gt                6794
_reflns_number_total             8413
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101547r_si_003.cif
_cod_data_source_block           ant014
_cod_original_cell_volume        53835(11)
_cod_database_code               4317311