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_4317310
_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_sum            'C38 H36 Br2 Cl N3 O6.13 U'
_chemical_formula_weight         1066.00
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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            8
_cell_length_a                   19.6629(4)
_cell_length_b                   19.6629(4)
_cell_length_c                   19.5797(4)
_cell_measurement_reflns_used    5887
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.70
_cell_measurement_theta_min      3.88
_cell_volume                     7570.1(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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  0.0647
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28228
_diffrn_reflns_theta_full        24.70
_diffrn_reflns_theta_max         24.70
_diffrn_reflns_theta_min         3.88
_exptl_absorpt_coefficient_mu    6.520
_exptl_absorpt_correction_T_max  0.7364
_exptl_absorpt_correction_T_min  0.4413
_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    1.871
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4104
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.015(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         6424
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+45.3899P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0586
_reflns_number_gt                5887
_reflns_number_total             6424
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101547r_si_002.cif
_cod_data_source_block           ant031
_cod_database_code               4317310