Syntheses and Characterization of Some Mixed Te/Se Polychalcogenide Anions [TemSen]2-
Perumal Sekar; James A. Ibers; Inorganic Chemistry 43 (2004) 5436–5441; doi:10.1021/ic040026h

data_4311808
_publ_section_title
;
 Syntheses and Characterization of Some Mixed Te/Se Polychalcogenide
 Anions [TemSen]2-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5436
_journal_page_last               5441
_journal_paper_doi               10.1021/ic040026h
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C11 H31 N3 O Se3 Te'
_chemical_formula_weight         585.87
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 107.9920(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.6014(10)
_cell_length_b                   11.7941(8)
_cell_length_c                   11.8795(8)
_cell_measurement_temperature    153(2)
_cell_volume                     2079.0(2)
_computing_cell_refinement       'SAINT (Bruker 2000)'
_computing_data_collection       'SMART (Bruker 2000)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'XP in SHELXTL'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2000)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.927
_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  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24019
_diffrn_reflns_theta_full        28.91
_diffrn_reflns_theta_max         28.91
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    6.682
_exptl_absorpt_correction_T_max  0.6684
_exptl_absorpt_correction_T_min  0.3321
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.872
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.206
_exptl_crystal_size_mid          0.172
_exptl_crystal_size_min          0.064
_refine_diff_density_max         1.314
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.242
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         5080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.242
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0706
_reflns_number_gt                4000
_reflns_number_total             5080
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic040026h_5.cif
_cod_data_source_block           '[NMe4]2[TeSe3].DMF_Compound5'
_cod_database_code               4311808