#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:50:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179157 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/18/4311810.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4311810
loop_
_publ_author_name
'Perumal Sekar'
'James A. Ibers'
_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            'C48 H40 P2 Se10 Te'
_chemical_formula_weight         1595.94
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           14
_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                 103.052(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.8811(12)
_cell_length_b                   14.0423(16)
_cell_length_c                   18.570(2)
_cell_measurement_temperature    153(2)
_cell_volume                     2510.1(5)
_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 0.483
_diffrn_measured_fraction_theta_max 0.483
_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  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0539
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       2
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            4882
_diffrn_reflns_theta_full        28.78
_diffrn_reflns_theta_max         28.78
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    7.941
_exptl_crystal_density_diffrn    2.112
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1500
_refine_diff_density_max         4.563
_refine_diff_density_min         -1.679
_refine_diff_density_rms         0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         3152
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0736
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1137P)²+44.1693P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1989
_refine_ls_wR_factor_ref         0.2190
_reflns_number_gt                2270
_reflns_number_total             3152
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic040026h_7.cif
_cod_data_source_block           jtese_[PPh4]2[TeSe10]
_cod_database_code               4311810
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Te1 Te 0.5000 0.5000 0.0000 0.0327(5) Uani 1 2 d S . .
Se1 Se 0.60579(17) 0.65251(13) 0.09373(7) 0.0291(5) Uani 1 1 d . . .
Se2 Se 0.53073(16) 0.60574(13) 0.19968(6) 0.0296(5) Uani 1 1 d . . .
Se3 Se 0.2993(2) 0.66612(15) 0.17936(7) 0.0386(6) Uani 1 1 d . . .
Se4 Se 0.1588(2) 0.54972(15) 0.10217(7) 0.0428(6) Uani 1 1 d . . .
Se5 Se 0.2166(2) 0.55748(16) -0.01354(8) 0.0490(7) Uani 1 1 d . . .
P1 P 1.2320(4) 0.4729(3) 0.39013(16) 0.0242(11) Uani 1 1 d . . .
C1 C 1.3563(15) 0.4018(12) 0.3594(6) 0.021(4) Uani 1 1 d . . .
C2 C 1.3606(18) 0.4034(13) 0.2841(6) 0.032(5) Uani 1 1 d . . .
H2A H 1.2962 0.4411 0.2501 0.038 Uiso 1 1 calc R . .
C3 C 1.458(2) 0.3507(16) 0.2603(8) 0.043(6) Uani 1 1 d . . .
H3A H 1.4597 0.3534 0.2095 0.052 Uiso 1 1 calc R . .
C4 C 1.555(2) 0.2924(13) 0.3073(8) 0.034(5) Uani 1 1 d . . .
H4A H 1.6230 0.2572 0.2897 0.041 Uiso 1 1 calc R . .
C5 C 1.5464(18) 0.2889(15) 0.3825(8) 0.040(5) Uani 1 1 d . . .
H5A H 1.6079 0.2484 0.4156 0.048 Uiso 1 1 calc R . .
C6 C 1.4547(17) 0.3408(13) 0.4078(7) 0.030(4) Uani 1 1 d . . .
H6A H 1.4538 0.3378 0.4588 0.036 Uiso 1 1 calc R . .
C7 C 1.2135(15) 0.4274(14) 0.4796(6) 0.029(5) Uani 1 1 d . . .
C8 C 1.1799(17) 0.3344(13) 0.4884(6) 0.028(4) Uani 1 1 d . . .
H8A H 1.1656 0.2919 0.4475 0.034 Uiso 1 1 calc R . .
C9 C 1.1666(17) 0.3019(13) 0.5573(7) 0.031(5) Uani 1 1 d . . .
H9A H 1.1418 0.2376 0.5637 0.037 Uiso 1 1 calc R . .
C10 C 1.190(2) 0.3653(17) 0.6172(7) 0.042(5) Uani 1 1 d . . .
H10A H 1.1852 0.3423 0.6646 0.050 Uiso 1 1 calc R . .
C11 C 1.2204(19) 0.4577(17) 0.6095(6) 0.044(6) Uani 1 1 d . . .
H11A H 1.2319 0.4988 0.6511 0.052 Uiso 1 1 calc R . .
C12 C 1.2352(17) 0.4953(14) 0.5403(7) 0.031(4) Uani 1 1 d . . .
H12A H 1.2576 0.5602 0.5343 0.038 Uiso 1 1 calc R . .
C13 C 1.2877(16) 0.5960(13) 0.3976(7) 0.027(4) Uani 1 1 d . . .
C14 C 1.1995(17) 0.6632(14) 0.4181(7) 0.035(5) Uani 1 1 d . . .
H14A H 1.1122 0.6445 0.4267 0.042 Uiso 1 1 calc R . .
C15 C 1.242(2) 0.7589(14) 0.4257(7) 0.038(5) Uani 1 1 d . . .
H15A H 1.1853 0.8066 0.4403 0.045 Uiso 1 1 calc R . .
C16 C 1.372(2) 0.7806(14) 0.4108(8) 0.039(5) Uani 1 1 d . . .
H16A H 1.4014 0.8450 0.4163 0.047 Uiso 1 1 calc R . .
C17 C 1.4563(18) 0.7176(14) 0.3896(7) 0.033(5) Uani 1 1 d . . .
H17A H 1.5418 0.7364 0.3787 0.040 Uiso 1 1 calc R . .
C18 C 1.4118(16) 0.6211(13) 0.3842(7) 0.029(4) Uani 1 1 d . . .
H18A H 1.4702 0.5735 0.3710 0.035 Uiso 1 1 calc R . .
C19 C 1.0690(16) 0.4626(13) 0.3213(6) 0.026(4) Uani 1 1 d . . .
C20 C 1.0331(17) 0.5391(13) 0.2701(7) 0.030(4) Uani 1 1 d . . .
H20A H 1.0883 0.5950 0.2737 0.036 Uiso 1 1 calc R . .
C21 C 0.9117(19) 0.5277(14) 0.2136(8) 0.038(5) Uani 1 1 d . . .
H21A H 0.8827 0.5782 0.1796 0.045 Uiso 1 1 calc R . .
C22 C 0.8346(16) 0.4453(14) 0.2067(7) 0.032(5) Uani 1 1 d . . .
H22A H 0.7550 0.4386 0.1673 0.038 Uiso 1 1 calc R . .
C23 C 0.8728(17) 0.3720(14) 0.2571(8) 0.035(5) Uani 1 1 d . . .
H23A H 0.8176 0.3160 0.2533 0.041 Uiso 1 1 calc R . .
C24 C 0.9936(18) 0.3805(13) 0.3141(8) 0.035(5) Uani 1 1 d . . .
H24A H 1.0224 0.3292 0.3474 0.042 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Se1 Te1 Se1 180.0 . 3_665 ?
Se1 Te1 Se5 93.39(5) . . ?
Se1 Te1 Se5 86.62(5) 3_665 . ?
Se1 Te1 Se5 86.62(5) . 3_665 ?
Se1 Te1 Se5 93.38(5) 3_665 3_665 ?
Se5 Te1 Se5 180.0 . 3_665 ?
Se2 Se1 Te1 99.34(7) . . ?
Se1 Se2 Se3 103.93(7) . . ?
Se2 Se3 Se4 104.88(10) . . ?
Se5 Se4 Se3 106.72(10) . . ?
Se4 Se5 Te1 109.95(8) . . ?
C1 P1 C13 110.0(8) . . ?
C1 P1 C19 107.2(6) . . ?
C13 P1 C19 109.6(7) . . ?
C1 P1 C7 108.3(7) . . ?
C13 P1 C7 110.9(7) . . ?
C19 P1 C7 110.8(8) . . ?
C2 C1 C6 117.4(14) . . ?
C2 C1 P1 119.2(11) . . ?
C6 C1 P1 123.4(11) . . ?
C3 C2 C1 119.6(13) . . ?
C3 C2 H2A 120.2 . . ?
C1 C2 H2A 120.2 . . ?
C2 C3 C4 123.3(14) . . ?
C2 C3 H3A 118.3 . . ?
C4 C3 H3A 118.3 . . ?
C3 C4 C5 116.4(18) . . ?
C3 C4 H4A 121.8 . . ?
C5 C4 H4A 121.8 . . ?
C6 C5 C4 121.8(15) . . ?
C6 C5 H5A 119.1 . . ?
C4 C5 H5A 119.1 . . ?
C5 C6 C1 121.4(13) . . ?
C5 C6 H6A 119.3 . . ?
C1 C6 H6A 119.3 . . ?
C8 C7 C12 122.0(13) . . ?
C8 C7 P1 121.4(10) . . ?
C12 C7 P1 116.6(14) . . ?
C7 C8 C9 119.9(14) . . ?
C7 C8 H8A 120.1 . . ?
C9 C8 H8A 120.1 . . ?
C8 C9 C10 119.2(18) . . ?
C8 C9 H9A 120.4 . . ?
C10 C9 H9A 120.4 . . ?
C11 C10 C9 121.9(14) . . ?
C11 C10 H10A 119.0 . . ?
C9 C10 H10A 119.0 . . ?
C10 C11 C12 121.5(15) . . ?
C10 C11 H11A 119.3 . . ?
C12 C11 H11A 119.3 . . ?
C11 C12 C7 115.4(18) . . ?
C11 C12 H12A 122.3 . . ?
C7 C12 H12A 122.3 . . ?
C18 C13 C14 121.5(17) . . ?
C18 C13 P1 120.5(14) . . ?
C14 C13 P1 118.0(14) . . ?
C13 C14 C15 119.0(17) . . ?
C13 C14 H14A 120.5 . . ?
C15 C14 H14A 120.5 . . ?
C14 C15 C16 116.9(18) . . ?
C14 C15 H15A 121.6 . . ?
C16 C15 H15A 121.6 . . ?
C17 C16 C15 125.0(18) . . ?
C17 C16 H16A 117.5 . . ?
C15 C16 H16A 117.5 . . ?
C16 C17 C18 116.6(17) . . ?
C16 C17 H17A 121.7 . . ?
C18 C17 H17A 121.7 . . ?
C13 C18 C17 121.0(17) . . ?
C13 C18 H18A 119.5 . . ?
C17 C18 H18A 119.5 . . ?
C24 C19 C20 121.6(12) . . ?
C24 C19 P1 120.9(11) . . ?
C20 C19 P1 117.1(13) . . ?
C21 C20 C19 116.9(16) . . ?
C21 C20 H20A 121.6 . . ?
C19 C20 H20A 121.6 . . ?
C22 C21 C20 121.6(15) . . ?
C22 C21 H21A 119.2 . . ?
C20 C21 H21A 119.2 . . ?
C21 C22 C23 120.1(12) . . ?
C21 C22 H22A 119.9 . . ?
C23 C22 H22A 119.9 . . ?
C22 C23 C24 119.9(17) . . ?
C22 C23 H23A 120.0 . . ?
C24 C23 H23A 120.0 . . ?
C19 C24 C23 119.8(15) . . ?
C19 C24 H24A 120.1 . . ?
C23 C24 H24A 120.1 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Te1 Se1 2.8085(16) . ?
Te1 Se1 2.8085(16) 3_665 ?
Te1 Se5 2.870(2) . ?
Te1 Se5 2.870(2) 3_665 ?
Se1 Se2 2.348(2) . ?
Se2 Se3 2.388(3) . ?
Se3 Se4 2.399(2) . ?
Se4 Se5 2.347(2) . ?
P1 C1 1.774(15) . ?
P1 C13 1.809(18) . ?
P1 C19 1.822(13) . ?
P1 C7 1.827(15) . ?
C1 C2 1.410(17) . ?
C1 C6 1.446(19) . ?
C2 C3 1.36(3) . ?
C2 H2A 0.9500 . ?
C3 C4 1.41(3) . ?
C3 H3A 0.9500 . ?
C4 C5 1.42(2) . ?
C4 H4A 0.9500 . ?
C5 C6 1.33(2) . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9500 . ?
C7 C8 1.37(2) . ?
C7 C12 1.46(2) . ?
C8 C9 1.39(2) . ?
C8 H8A 0.9500 . ?
C9 C10 1.40(2) . ?
C9 H9A 0.9500 . ?
C10 C11 1.35(3) . ?
C10 H10A 0.9500 . ?
C11 C12 1.43(2) . ?
C11 H11A 0.9500 . ?
C12 H12A 0.9500 . ?
C13 C18 1.35(2) . ?
C13 C14 1.39(2) . ?
C14 C15 1.40(3) . ?
C14 H14A 0.9500 . ?
C15 C16 1.40(3) . ?
C15 H15A 0.9500 . ?
C16 C17 1.34(3) . ?
C16 H16A 0.9500 . ?
C17 C18 1.42(2) . ?
C17 H17A 0.9500 . ?
C18 H18A 0.9500 . ?
C19 C24 1.36(2) . ?
C19 C20 1.43(2) . ?
C20 C21 1.413(19) . ?
C20 H20A 0.9500 . ?
C21 C22 1.38(2) . ?
C21 H21A 0.9500 . ?
C22 C23 1.38(2) . ?
C22 H22A 0.9500 . ?
C23 C24 1.410(18) . ?
C23 H23A 0.9500 . ?
C24 H24A 0.9500 . ?
