Tris(tetrabutylammonium) tris(nitrato-κ^2^<i>O</i>,<i>O</i>')tetrakis(thiocyanato-κ<i>N</i>)thorium(IV)
Lozano-Rodriguez, M. Janeth; Thuéry, Pierre; Petit, Sébastien; Copping, Roy; Mustre de Leon, Jose; Den Auwer, Christophe; Acta Crystallographica Section E 67 (2011) m487–; doi:10.1107/S1600536811009792

data_2229859
_publ_section_title
;
 Tris(tetrabutylammonium)
 tris(nitrato-\k^2^<i>O</i>,<i>O</i>')tetrakis(thiocyanato-\k<i>N</i>)thorium(IV)
;
_journal_coeditor_code           TK2728
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m487
_journal_paper_doi               10.1107/S1600536811009792
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '(C16 H36 N)3 [Th (N C S)4 (N O3)3]'
_chemical_formula_moiety         '3(C16 H36 N +), C4 N7 O9 S4 Th 3-'
_chemical_formula_sum            'C52 H108 N10 O9 S4 Th'
_chemical_formula_weight         1377.76
_chemical_name_systematic
;
Tris(tetrabutylammonium)
tris(nitrato-\k^2^<i>O</i>,<i>O</i>')tetrakis(thiocyanato-\k<i>N</i>)thorium(IV)
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.946(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.1057(7)
_cell_length_b                   17.5943(8)
_cell_length_c                   16.7084(8)
_cell_measurement_reflns_used    170199
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      3.19
_cell_volume                     3539.6(3)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method
'two \f and eleven \w scans with 2\% steps (649 frames)'
_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  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            170199
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         4.10
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.276
_exptl_absorpt_correction_T_max  0.853
_exptl_absorpt_correction_T_min  0.703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.983
_refine_diff_density_min         -0.757
_refine_ls_abs_structure_details 'Flack (1983), 6435 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.008(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         13392
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+4.0973P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0890
_reflns_number_gt                11074
_reflns_number_total             13392
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk2728.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2229859
_cod_database_fobs_code          2229859