#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/91/4309198.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_4309198
loop_
_publ_author_name
'Jari Konu'
'Markku Ahlgrén'
'Stephen M. Aucott'
'Tristram Chivers'
'Sophie H. Dale'
'Mark R. J. Elsegood'
'Kathryn E. Holmes'
'Sarah L. M. James'
'Paul F. Kelly'
'Risto S. Laitinen'
_publ_section_title
;
Synthetic Applications of (Me3SiNSN)2E (E = S, Se) in Chalcogen-Nitrogen
Chemistry: Formation and Structural Characterization of Cl2TeESN2 (E = S,
Se) and [PPh4]2[Pd2(μ-Se2N2S)X4] (X = Cl, Br)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4992
_journal_page_last               5000
_journal_paper_doi               10.1021/ic050261f
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'Cl2 N2 S Se Te'
_chemical_formula_weight         337.54
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c 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            8
_cell_length_a                   8.3524(17)
_cell_length_b                   7.9527(16)
_cell_length_c                   19.853(4)
_cell_measurement_temperature    150(2)
_cell_volume                     1318.7(5)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'DIAMOND (Brandenburg & Berndt, 1999)'
_computing_publication_material  'WINGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Nonius Kappaccd'
_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  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0179
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13311
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    11.039
_exptl_absorpt_correction_T_max  0.4048
_exptl_absorpt_correction_T_min  0.2162
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.404
_refine_diff_density_min         -2.313
_refine_diff_density_rms         0.277
_refine_ls_extinction_coef       0.0018(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     65
_refine_ls_number_reflns         1150
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0597P)²+31.6007P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1260
_reflns_number_gt                1131
_reflns_number_total             1150
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050261fsi20050219_081655_2.cif
_cod_data_source_block           cmpd2
_cod_database_code               4309198
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -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 0.39350(7) 0.06797(8) 0.08914(3) 0.0144(3) Uani 1 1 d . . .
Se1 Se 0.49285(14) 0.17522(16) 0.20167(6) 0.0315(4) Uani 1 1 d . . .
S1 S 0.7541(3) 0.0467(3) 0.11864(13) 0.0232(6) Uani 1 1 d . . .
N2 N 0.6980(11) 0.1312(12) 0.1845(4) 0.026(2) Uani 1 1 d . . .
N1 N 0.6182(10) 0.0013(11) 0.0680(4) 0.0173(17) Uani 1 1 d . . .
Cl1 Cl 0.4424(3) 0.3310(3) 0.03155(12) 0.0226(6) Uani 1 1 d . . .
Cl2 Cl 0.3720(3) -0.2453(3) 0.14944(12) 0.0211(6) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Te1 0.0146(4) 0.0156(4) 0.0129(4) -0.0007(2) 0.0013(2) -0.0025(2)
Se1 0.0276(7) 0.0383(7) 0.0287(7) -0.0055(5) -0.0005(5) 0.0005(5)
S1 0.0151(12) 0.0286(13) 0.0260(13) -0.0050(11) 0.0031(11) 0.0015(10)
N2 0.018(4) 0.038(5) 0.024(4) -0.001(4) -0.003(4) 0.001(4)
N1 0.017(4) 0.019(4) 0.016(4) 0.001(3) 0.003(3) -0.004(3)
Cl1 0.0270(13) 0.0201(12) 0.0207(11) 0.0047(9) 0.0011(10) -0.0057(10)
Cl2 0.0185(12) 0.0232(12) 0.0214(11) 0.0062(10) -0.0025(9) -0.0011(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
N1 Te1 Cl1 88.4(2) . . ?
N1 Te1 Se1 88.1(2) . . ?
Cl1 Te1 Se1 94.05(7) . . ?
N1 Te1 Cl2 85.0(2) . . ?
Cl1 Te1 Cl2 173.31(8) . . ?
Se1 Te1 Cl2 86.72(6) . . ?
N2 Se1 Te1 94.6(3) . . ?
N2 S1 N1 115.2(5) . . ?
S1 N2 Se1 122.6(5) . . ?
S1 N1 Te1 119.2(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 N1 1.994(8) . ?
Te1 Cl1 2.418(2) . ?
Te1 Se1 2.5313(13) . ?
Te1 Cl2 2.770(2) . ?
Se1 N2 1.781(9) . ?
S1 N2 1.543(9) . ?
S1 N1 1.558(9) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Te1 Se1 N2 3.3(4) . . . . ?
Cl1 Te1 Se1 N2 -84.9(3) . . . . ?
Cl2 Te1 Se1 N2 88.4(3) . . . . ?
N1 S1 N2 Se1 -0.4(9) . . . . ?
Te1 Se1 N2 S1 -2.3(7) . . . . ?
N2 S1 N1 Te1 4.1(8) . . . . ?
Cl1 Te1 N1 S1 89.7(5) . . . . ?
Se1 Te1 N1 S1 -4.4(5) . . . . ?
Cl2 Te1 N1 S1 -91.3(5) . . . . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30660858
