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_4317313
_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_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C32 H24 Cl N2 O6 S U, C4 H12 N'
_chemical_formula_sum            'C36 H36 Cl N3 O6 S U'
_chemical_formula_weight         912.24
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      82
_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_date             2009-02-17T11:53:52-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.9226(2)
_cell_length_b                   18.9226(2)
_cell_length_c                   19.5451(4)
_cell_measurement_reflns_used    31034
_cell_measurement_temperature    173.0(1)
_cell_measurement_theta_max      27.103
_cell_measurement_theta_min      0.407
_cell_measurement_wavelength     0.71073
_cell_volume                     6998.41(18)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_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-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.257976E-1
_diffrn_orient_matrix_UB_12      0.374807E-1
_diffrn_orient_matrix_UB_13      -0.260228E-1
_diffrn_orient_matrix_UB_21      -0.445603E-1
_diffrn_orient_matrix_UB_22      0.123068E-1
_diffrn_orient_matrix_UB_23      -0.247913E-1
_diffrn_orient_matrix_UB_31      -0.119017E-1
_diffrn_orient_matrix_UB_32      0.351644E-1
_diffrn_orient_matrix_UB_33      0.364134E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19105
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.58
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    4.824
_exptl_absorpt_correction_T_max  0.512
_exptl_absorpt_correction_T_min  0.383
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs2002 (Sheldrick, 2002)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3568
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.587
_refine_diff_density_min         -0.42
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.037(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.059
_refine_ls_wR_factor_ref         0.061
_reflns_number_gt                5507
_reflns_number_total             6060
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101547r_si_005.cif
_cod_data_source_block           7(TMA)Cl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_formula_sum        'C36 H36 Cl N3 O6 S U '
_cod_database_code               4317313