#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:50:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179157 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/18/4311804.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_4311804
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            'C16 H40 N2 Se6 Te3'
_chemical_formula_weight         1117.06
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.4975(8)
_cell_length_b                   13.1068(7)
_cell_length_c                   15.8270(8)
_cell_measurement_temperature    153(2)
_cell_volume                     3007.4(3)
_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 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Bruker 1000 CCD'
_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  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34894
_diffrn_reflns_theta_full        28.95
_diffrn_reflns_theta_max         28.95
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    10.160
_exptl_crystal_density_diffrn    2.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2040
_refine_diff_density_max         1.706
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.274
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3961
_refine_ls_number_restraints     154
_refine_ls_restrained_S_all      1.264
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
   [1.00000+0.00000exp(0.00(sinθ/λ)²)]/
     [σ²(Fo²)+0.0000+0.0000*P+(0.0300P)²+0.0000sinθ/λ]
   where P = 1.00000Fo² + 0.00000Fc²
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0564
_refine_ls_wR_factor_ref         0.0601
_reflns_number_gt                3328
_reflns_number_total             3961
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic040026h_1.cif
_cod_data_source_block           jte3se6_compound1
_cod_database_code               4311804
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, 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 0.929664(15) 0.007113(17) 1.635913(16) 0.03420(7) Uani 0.50 1 d P . .
Te2 Te 0.510680(16) 0.2500 1.753224(15) 0.02424(7) Uani 1 2 d S . .
Te3 Te 0.773882(14) 0.2500 1.669455(14) 0.01961(6) Uani 1 2 d S . .
Se1 Se 0.929664(15) 0.007113(17) 1.635913(16) 0.03420(7) Uani 0.50 1 d P . .
Se2 Se 0.76796(2) 0.03655(2) 1.66851(2) 0.03331(8) Uani 1 1 d . . .
Se3 Se 0.60737(2) 0.2500 1.61816(2) 0.03142(10) Uani 1 2 d S . .
Se4 Se 0.51622(2) 0.03991(2) 1.73548(2) 0.03718(9) Uani 1 1 d . . .
N1 N 0.8059(2) 0.2500 1.37194(18) 0.0218(6) Uani 1 2 d SDU . .
C1 C 0.8600(4) 0.1884(4) 1.3062(3) 0.0283(11) Uani 0.50 1 d PDU A -1
H1A H 0.8915 0.1315 1.3355 0.034 Uiso 0.50 1 calc PR A -1
H1B H 0.8156 0.1582 1.2658 0.034 Uiso 0.50 1 calc PR A -1
C2 C 0.7485(3) 0.1760(4) 1.4241(3) 0.0272(11) Uani 0.50 1 d PDU A -1
H2A H 0.7900 0.1226 1.4466 0.033 Uiso 0.50 1 calc PR A -1
H2B H 0.7227 0.2135 1.4729 0.033 Uiso 0.50 1 calc PR A -1
C3 C 0.8709(3) 0.3071(4) 1.4303(3) 0.0267(11) Uani 0.50 1 d PDU A -1
H3A H 0.9001 0.3629 1.3978 0.032 Uiso 0.50 1 calc PR A -1
H3B H 0.8339 0.3388 1.4758 0.032 Uiso 0.50 1 calc PR A -1
C4 C 0.7450(4) 0.3270(5) 1.3273(4) 0.0342(13) Uani 0.50 1 d PDU A -1
H4A H 0.7854 0.3763 1.2977 0.041 Uiso 0.50 1 calc PR A -1
H4B H 0.7091 0.2904 1.2835 0.041 Uiso 0.50 1 calc PR A -1
C5 C 0.9308(3) 0.2472(15) 1.2570(3) 0.0343(14) Uani 1 2 d SDU A -1
H5A H 0.9608 0.2018 1.2162 0.051 Uiso 0.50 1 calc PR A -1
H5B H 0.9772 0.2748 1.2959 0.051 Uiso 0.50 1 calc PR A -1
H5C H 0.9006 0.3034 1.2269 0.051 Uiso 0.50 1 calc PR A -1
C6 C 0.6704(14) 0.1245(18) 1.3783(11) 0.038(4) Uani 0.50 1 d PDU A -1
H6A H 0.6379 0.0788 1.4172 0.058 Uiso 0.50 1 calc PR A -1
H6B H 0.6950 0.0849 1.3308 0.058 Uiso 0.50 1 calc PR A -1
H6C H 0.6275 0.1762 1.3570 0.058 Uiso 0.50 1 calc PR A -1
C7 C 0.9462(3) 0.245(2) 1.4707(3) 0.0378(17) Uani 0.50 1 d PDU A -1
H7A H 0.9841 0.2886 1.5066 0.057 Uiso 0.50 1 calc PR A -1
H7B H 0.9848 0.2141 1.4265 0.057 Uiso 0.50 1 calc PR A -1
H7C H 0.9185 0.1904 1.5050 0.057 Uiso 0.50 1 calc PR A -1
C8 C 0.6788(15) 0.386(2) 1.3813(13) 0.048(5) Uani 0.50 1 d PDU A -1
H8A H 0.6441 0.4338 1.3460 0.072 Uiso 0.50 1 calc PR A -1
H8B H 0.7131 0.4238 1.4244 0.072 Uiso 0.50 1 calc PR A -1
H8C H 0.6360 0.3386 1.4088 0.072 Uiso 0.50 1 calc PR A -1
N2 N 0.79188(19) 0.2500 0.97659(18) 0.0239(6) Uani 1 2 d SDU . .
C9 C 0.7630(4) 0.1846(4) 0.9030(3) 0.0291(12) Uani 0.50 1 d PDU B -1
H9A H 0.8177 0.1469 0.8823 0.035 Uiso 0.50 1 calc PR B -1
H9B H 0.7418 0.2297 0.8568 0.035 Uiso 0.50 1 calc PR B -1
C10 C 0.8268(3) 0.1901(4) 1.0500(3) 0.0273(11) Uani 0.50 1 d PDU B -1
H10A H 0.7767 0.1448 1.0702 0.033 Uiso 0.50 1 calc PR B -1
H10B H 0.8417 0.2379 1.0964 0.033 Uiso 0.50 1 calc PR B -1
C11 C 0.7099(3) 0.3149(4) 1.0091(3) 0.0287(11) Uani 0.50 1 d PDU B -1
H11A H 0.6633 0.2683 1.0337 0.034 Uiso 0.50 1 calc PR B -1
H11B H 0.7325 0.3595 1.0552 0.034 Uiso 0.50 1 calc PR B -1
C12 C 0.8661(3) 0.3236(4) 0.9428(3) 0.0307(11) Uani 0.50 1 d PDU B -1
H12A H 0.9163 0.2824 0.9176 0.037 Uiso 0.50 1 calc PR B -1
H12B H 0.8384 0.3647 0.8968 0.037 Uiso 0.50 1 calc PR B -1
C13 C 0.6878(6) 0.1088(8) 0.9221(7) 0.033(2) Uani 0.50 1 d PDU B -1
H13A H 0.6730 0.0702 0.8708 0.049 Uiso 0.50 1 calc PR B -1
H13B H 0.6327 0.1451 0.9417 0.049 Uiso 0.50 1 calc PR B -1
H13C H 0.7088 0.0618 0.9662 0.049 Uiso 0.50 1 calc PR B -1
C14 C 0.9111(8) 0.1255(9) 1.0319(7) 0.037(2) Uani 0.50 1 d PDU B -1
H14A H 0.9302 0.0903 1.0836 0.055 Uiso 0.50 1 calc PR B -1
H14B H 0.9614 0.1694 1.0121 0.055 Uiso 0.50 1 calc PR B -1
H14C H 0.8963 0.0751 0.9882 0.055 Uiso 0.50 1 calc PR B -1
C15 C 0.6630(7) 0.3809(10) 0.9435(7) 0.040(2) Uani 0.50 1 d PDU B -1
H15A H 0.6116 0.4178 0.9697 0.060 Uiso 0.50 1 calc PR B -1
H15B H 0.6396 0.3378 0.8977 0.060 Uiso 0.50 1 calc PR B -1
H15C H 0.7075 0.4300 0.9206 0.060 Uiso 0.50 1 calc PR B -1
C16 C 0.9081(9) 0.3953(8) 1.0057(6) 0.039(2) Uani 0.50 1 d PDU B -1
H16A H 0.9540 0.4382 0.9774 0.058 Uiso 0.50 1 calc PR B -1
H16B H 0.9379 0.3560 1.0507 0.058 Uiso 0.50 1 calc PR B -1
H16C H 0.8597 0.4385 1.0300 0.058 Uiso 0.50 1 calc PR B -1
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'
N N 0.0061 0.0033 '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
Se4 Te1 Se2 106.986(14) 6_659 . ?
Se3 Te2 Se4 84.219(8) . . ?
Se3 Te2 Se4 84.221(8) . 7_565 ?
Se4 Te2 Se4 167.890(17) . 7_565 ?
Se3 Te3 Se2 88.236(7) . 7_565 ?
Se3 Te3 Se2 88.236(7) . . ?
Se2 Te3 Se2 176.431(14) 7_565 . ?
Te1 Se2 Te3 97.480(12) . . ?
Te3 Se3 Te2 104.665(15) . . ?
Se1 Se4 Te1 0.000(14) 6_559 6_559 ?
Se1 Se4 Te2 94.359(12) 6_559 . ?
Te1 Se4 Te2 94.359(12) 6_559 . ?
C4 N1 C4 83.5(5) 7_565 . ?
C4 N1 C3 167.0(3) 7_565 . ?
C4 N1 C3 108.5(3) . . ?
C4 N1 C3 108.5(3) 7_565 7_565 ?
C4 N1 C3 167.0(4) . 7_565 ?
C3 N1 C3 59.1(4) . 7_565 ?
C4 N1 C2 111.1(4) 7_565 7_565 ?
C4 N1 C2 60.7(3) . 7_565 ?
C3 N1 C2 72.2(3) . 7_565 ?
C3 N1 C2 108.9(3) 7_565 7_565 ?
C4 N1 C2 60.7(3) 7_565 . ?
C4 N1 C2 111.1(4) . . ?
C3 N1 C2 108.9(3) . . ?
C3 N1 C2 72.3(3) 7_565 . ?
C2 N1 C2 79.2(5) 7_565 . ?
C4 N1 C1 109.4(3) 7_565 7_565 ?
C4 N1 C1 68.4(3) . 7_565 ?
C3 N1 C1 80.5(3) . 7_565 ?
C3 N1 C1 110.8(3) 7_565 7_565 ?
C2 N1 C1 108.2(3) 7_565 7_565 ?
C2 N1 C1 169.7(3) . 7_565 ?
C4 N1 C1 68.4(3) 7_565 . ?
C4 N1 C1 109.4(3) . . ?
C3 N1 C1 110.8(3) . . ?
C3 N1 C1 80.5(3) 7_565 . ?
C2 N1 C1 169.7(3) 7_565 . ?
C2 N1 C1 108.2(3) . . ?
C1 N1 C1 63.5(4) 7_565 . ?
C5 C1 N1 115.6(7) . . ?
C6 C2 N1 115.9(8) . . ?
C7 C3 N1 116.1(8) . . ?
C8 C4 N1 116.7(9) . . ?
C10 N2 C10 63.6(4) 7_565 . ?
C10 N2 C9 113.4(3) 7_565 7_565 ?
C10 N2 C9 175.7(3) . 7_565 ?
C10 N2 C9 175.7(3) 7_565 . ?
C10 N2 C9 113.4(3) . . ?
C9 N2 C9 69.4(5) 7_565 . ?
C10 N2 C12 72.8(3) 7_565 . ?
C10 N2 C12 111.3(3) . . ?
C9 N2 C12 64.5(3) 7_565 . ?
C9 N2 C12 106.4(3) . . ?
C10 N2 C12 111.3(3) 7_565 7_565 ?
C10 N2 C12 72.8(3) . 7_565 ?
C9 N2 C12 106.4(3) 7_565 7_565 ?
C9 N2 C12 64.5(3) . 7_565 ?
C12 N2 C12 77.5(4) . 7_565 ?
C10 N2 C11 73.3(3) 7_565 . ?
C10 N2 C11 106.9(3) . . ?
C9 N2 C11 74.4(3) 7_565 . ?
C9 N2 C11 110.9(3) . . ?
C12 N2 C11 107.9(3) . . ?
C12 N2 C11 174.0(3) 7_565 . ?
C10 N2 C11 106.9(3) 7_565 7_565 ?
C10 N2 C11 73.3(3) . 7_565 ?
C9 N2 C11 110.9(3) 7_565 7_565 ?
C9 N2 C11 74.4(3) . 7_565 ?
C12 N2 C11 174.0(3) . 7_565 ?
C12 N2 C11 107.9(3) 7_565 7_565 ?
C11 N2 C11 66.6(4) . 7_565 ?
N2 C9 C13 115.0(5) . . ?
N2 C10 C14 114.8(6) . . ?
C15 C11 N2 115.5(5) . . ?
C16 C12 N2 116.5(5) . . ?
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 Se4 2.4295(4) 6_659 ?
Te1 Se2 2.4312(4) . ?
Te2 Se3 2.5563(4) . ?
Te2 Se4 2.7690(4) . ?
Te2 Se4 2.7690(4) 7_565 ?
Te3 Se3 2.5469(4) . ?
Te3 Se2 2.7989(3) 7_565 ?
Te3 Se2 2.7990(3) . ?
Se4 Se1 2.4295(4) 6_559 ?
Se4 Te1 2.4295(4) 6_559 ?
N1 C4 1.515(5) 7_565 ?
N1 C4 1.515(5) . ?
N1 C3 1.517(5) . ?
N1 C3 1.517(5) 7_565 ?
N1 C2 1.521(5) 7_565 ?
N1 C2 1.521(5) . ?
N1 C1 1.533(5) 7_565 ?
N1 C1 1.533(5) . ?
C1 C5 1.500(11) . ?
C2 C6 1.504(12) . ?
C3 C7 1.506(13) . ?
C4 C8 1.500(13) . ?
N2 C10 1.491(5) 7_565 ?
N2 C10 1.491(5) . ?
N2 C9 1.506(5) 7_565 ?
N2 C9 1.506(5) . ?
N2 C12 1.541(5) . ?
N2 C12 1.541(5) 7_565 ?
N2 C11 1.549(5) . ?
N2 C11 1.549(5) 7_565 ?
C9 C13 1.505(9) . ?
C10 C14 1.515(9) . ?
C11 C15 1.513(10) . ?
C12 C16 1.497(10) . ?
