Tetraalkylammonium Uranyl Isothiocyanates
Clare E. Rowland; Mercouri G. Kanatzidis; L. Soderholm; Inorganic Chemistry 51 (2012) 11798–11804; doi:10.1021/ic301741u

data_4330910
_publ_contact_author_address
;Department of Chemistry
Northwestern University 
2145 Sheridan Rd. 
Evanston, IL 60208
;
_publ_contact_author_email       m-kanatzidis@northwestern.edu
_publ_contact_author_name        'Mercouri G. Kanatzidis'
_publ_section_title
;
 Tetraalkylammonium Uranyl Isothiocyanates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11798
_journal_page_last               11804
_journal_paper_doi               10.1021/ic301741u
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         '3(C8 H20 N), C5 N5 O2 S5 U'
_chemical_formula_sum            'C29 H60 N8 O2 S5 U'
_chemical_formula_weight         951.23
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 101.603(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.581(3)
_cell_length_b                   20.318(3)
_cell_length_c                   20.589(3)
_cell_measurement_reflns_used    9979
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.42
_cell_measurement_theta_min      4.1615
_cell_volume                     8434(2)
_computing_cell_refinement       'ApexII software suite (Bruker AXS)'
_computing_data_collection       'ApexII software suite (Bruker AXS)'
_computing_data_reduction        'ApexII software suite (Bruker AXS)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'omega scans'
_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  0.0770
_diffrn_reflns_av_sigmaI/netI    0.0626
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            66260
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         4.01
_exptl_absorpt_coefficient_mu    4.131
_exptl_absorpt_correction_T_max  0.662
_exptl_absorpt_correction_T_min  0.349
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_description       block
_exptl_crystal_F_000             3824
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.535
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     812
_refine_ls_number_reflns         15390
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0424P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0974
_reflns_number_gt                12546
_reflns_number_total             15390
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301741u_si_002_3.cif
_cod_data_source_block           2
_cod_original_cell_volume        8433.7(19)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4330910