#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:39:16 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179929 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/24/7022441.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_7022441
loop_
_publ_author_name
'Jolleys, Andrew'
'Levason, William'
'Reid, Gillian'
_publ_section_title
;
 Thioether coordination to divalent selenium halide acceptors--synthesis,
 properties and structures.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2963
_journal_page_last               2972
_journal_paper_doi               10.1039/c2dt32665e
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         '2(C16 H19 S4 1+), Cl6 Se 2-, 1.76(Cl2 Se)'
_chemical_formula_sum            'C32 H38 Cl9.52 S8 Se2.76'
_chemical_formula_weight         1234.52
_chemical_name_systematic
;
bis[3,4-bis(methylsulfanyl)phenyl](methyl)[2-(methylsulfanyl)phenyl]sulfonium
hexachloroselenate(IV) dichloroselenium(II)
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-10-27
_audit_creation_method           'SHELXL-97 + hand edit'
_cell_angle_alpha                112.040(8)
_cell_angle_beta                 96.489(7)
_cell_angle_gamma                92.494(7)
_cell_formula_units_Z            1
_cell_length_a                   10.095(4)
_cell_length_b                   10.111(4)
_cell_length_c                   12.633(5)
_cell_measurement_reflns_used    8152
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     1182.4(8)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       'Four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 '
_diffrn_measurement_method       'Profile data from ω-scans'
_diffrn_radiation_collimation    'Confocal mirrors, VHF VariMax '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_sigmaI/netI    0.0793
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10466
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.04
_diffrn_source                   'Rotating anode X-ray tube'
_diffrn_source_type              'Rigaku FR-E+ Superbright'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.065
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.499
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;Jacobson, R.A. (1998). REQAB. Private communication to the
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             613.7
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.313
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         5314
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0183P)²+3.7721P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1100
_reflns_number_gt                3902
_reflns_number_total             5314
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            c2dt32665e.txt
_cod_data_source_block           12aj012r
_cod_original_cell_volume        1182.5(8)
_cod_database_code               7022441
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
S1 S 0.81068(11) 0.53998(12) 0.27377(10) 0.0163(2) Uani 1 1 d .
S2 S 0.6846(2) 0.5133(2) 0.03865(14) 0.0607(6) Uani 1 1 d .
S3 S 0.32102(12) 0.59074(13) 0.42534(11) 0.0217(3) Uani 1 1 d .
S4 S 0.26552(12) 0.26727(13) 0.33542(11) 0.0213(3) Uani 1 1 d .
C1 C 0.9130(5) 0.5302(5) 0.3958(4) 0.0212(10) Uani 1 1 d .
H1A H 0.9014 0.4328 0.3945 0.032 Uiso 1 1 calc R
H1B H 0.8862 0.5981 0.4670 0.032 Uiso 1 1 calc R
H1C H 1.0071 0.5544 0.3927 0.032 Uiso 1 1 calc R
C2 C 0.8704(5) 0.4107(5) 0.1532(4) 0.0196(10) Uani 1 1 d .
C3 C 0.8161(5) 0.4066(6) 0.0439(4) 0.0282(12) Uani 1 1 d .
C4 C 0.8659(6) 0.3131(7) -0.0521(5) 0.0375(14) Uani 1 1 d .
H4 H 0.8312 0.3073 -0.1270 0.045 Uiso 1 1 calc R
C5 C 0.9652(6) 0.2290(6) -0.0393(5) 0.0392(15) Uani 1 1 d .
H5 H 1.0001 0.1677 -0.1054 0.047 Uiso 1 1 calc R
C6 C 1.0146(6) 0.2325(7) 0.0681(5) 0.0392(14) Uani 1 1 d .
H6 H 1.0816 0.1722 0.0754 0.047 Uiso 1 1 calc R
C7 C 0.9674(5) 0.3227(6) 0.1642(4) 0.0269(11) Uani 1 1 d .
H7 H 1.0011 0.3248 0.2382 0.032 Uiso 1 1 calc R
C8 C 0.6824(7) 0.5310(8) -0.0962(6) 0.0533(18) Uani 1 1 d .
H8A H 0.7724 0.5643 -0.1032 0.080 Uiso 1 1 calc R
H8B H 0.6198 0.6006 -0.1009 0.080 Uiso 1 1 calc R
H8C H 0.6538 0.4379 -0.1587 0.080 Uiso 1 1 calc R
C9 C 0.6552(4) 0.4556(5) 0.2825(4) 0.0173(9) Uani 1 1 d .
C10 C 0.5638(4) 0.5465(5) 0.3398(4) 0.0159(9) Uani 1 1 d .
H10 H 0.5827 0.6475 0.3671 0.019 Uiso 1 1 calc R
C11 C 0.4446(4) 0.4878(5) 0.3565(4) 0.0166(9) Uani 1 1 d .
C12 C 0.4181(5) 0.3352(5) 0.3107(4) 0.0180(10) Uani 1 1 d .
C13 C 0.5096(5) 0.2488(5) 0.2515(4) 0.0227(10) Uani 1 1 d .
H13 H 0.4898 0.1477 0.2197 0.027 Uiso 1 1 calc R
C14 C 0.6294(5) 0.3074(5) 0.2380(4) 0.0215(10) Uani 1 1 d .
H14 H 0.6930 0.2477 0.1989 0.026 Uiso 1 1 calc R
C15 C 0.3926(5) 0.7719(5) 0.4671(4) 0.0233(11) Uani 1 1 d .
H15A H 0.4761 0.7877 0.5198 0.035 Uiso 1 1 calc R
H15B H 0.3294 0.8384 0.5059 0.035 Uiso 1 1 calc R
H15C H 0.4114 0.7884 0.3984 0.035 Uiso 1 1 calc R
C16 C 0.2688(5) 0.0769(5) 0.2651(4) 0.0271(12) Uani 1 1 d .
H16A H 0.2737 0.0520 0.1830 0.041 Uiso 1 1 calc R
H16B H 0.1872 0.0282 0.2740 0.041 Uiso 1 1 calc R
H16C H 0.3472 0.0465 0.3001 0.041 Uiso 1 1 calc R
Se1 Se 0.0000 0.0000 0.5000 0.01462(15) Uani 1 2 d S
Cl1 Cl 0.22863(11) 0.10631(12) 0.54751(10) 0.0214(3) Uani 1 1 d .
Cl2 Cl 0.05058(12) -0.13186(12) 0.62240(10) 0.0231(3) Uani 1 1 d .
Cl3 Cl -0.06218(11) 0.19194(12) 0.66028(10) 0.0199(2) Uani 1 1 d .
Se2 Se 0.29029(6) 0.07076(6) 0.77369(5) 0.02282(15) Uani 0.80 1 d P
Cl4 Cl 0.2904(2) 0.03603(18) 0.93623(15) 0.0457(4) Uani 0.80 1 d P
Cl5 Cl 0.48299(18) 0.19255(18) 0.81688(18) 0.0477(5) Uani 0.80 1 d P
Se3 Se 0.4706(7) 0.2124(7) 0.9850(6) 0.0289(15) Uani 0.08 1 d P
Cl6 Cl 0.2904(2) 0.03603(18) 0.93623(15) 0.0457(4) Uani 0.08 1 d P
Cl7 Cl 0.48299(18) 0.19255(18) 0.81688(18) 0.0477(5) Uani 0.08 1 d P
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'
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'
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
C2 S1 C9 104.1(2) . .
C2 S1 C1 103.8(2) . .
C9 S1 C1 100.4(2) . .
C3 S2 C8 104.6(3) . .
C11 S3 C15 103.4(2) . .
C12 S4 C16 102.9(2) . .
S1 C1 H1A 109.5 . .
S1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
S1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
C7 C2 C3 121.2(5) . .
C7 C2 S1 122.9(4) . .
C3 C2 S1 115.9(4) . .
C4 C3 C2 117.7(5) . .
C4 C3 S2 124.8(4) . .
C2 C3 S2 117.5(4) . .
C5 C4 C3 120.4(5) . .
C5 C4 H4 119.8 . .
C3 C4 H4 119.8 . .
C4 C5 C6 120.9(5) . .
C4 C5 H5 119.6 . .
C6 C5 H5 119.6 . .
C7 C6 C5 120.1(5) . .
C7 C6 H6 119.9 . .
C5 C6 H6 119.9 . .
C6 C7 C2 119.7(5) . .
C6 C7 H7 120.2 . .
C2 C7 H7 120.2 . .
S2 C8 H8A 109.5 . .
S2 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
S2 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C14 C9 C10 122.1(4) . .
C14 C9 S1 121.5(4) . .
C10 C9 S1 116.3(3) . .
C11 C10 C9 119.3(4) . .
C11 C10 H10 120.3 . .
C9 C10 H10 120.3 . .
C10 C11 C12 118.5(4) . .
C10 C11 S3 123.6(4) . .
C12 C11 S3 117.8(3) . .
C13 C12 C11 120.4(4) . .
C13 C12 S4 123.3(4) . .
C11 C12 S4 116.3(4) . .
C14 C13 C12 120.9(4) . .
C14 C13 H13 119.6 . .
C12 C13 H13 119.6 . .
C13 C14 C9 118.7(4) . .
C13 C14 H14 120.6 . .
C9 C14 H14 120.6 . .
S3 C15 H15A 109.5 . .
S3 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
S3 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
S4 C16 H16A 109.5 . .
S4 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
S4 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
Cl3 Se1 Cl3 180.00(5) 2_556 .
Cl3 Se1 Cl1 90.52(4) 2_556 2_556
Cl3 Se1 Cl1 89.48(4) . 2_556
Cl3 Se1 Cl1 89.48(4) 2_556 .
Cl3 Se1 Cl1 90.52(4) . .
Cl1 Se1 Cl1 180.0 2_556 .
Cl3 Se1 Cl2 89.77(5) 2_556 2_556
Cl3 Se1 Cl2 90.23(5) . 2_556
Cl1 Se1 Cl2 89.79(4) 2_556 2_556
Cl1 Se1 Cl2 90.21(4) . 2_556
Cl3 Se1 Cl2 90.23(5) 2_556 .
Cl3 Se1 Cl2 89.77(5) . .
Cl1 Se1 Cl2 90.21(4) 2_556 .
Cl1 Se1 Cl2 89.79(4) . .
Cl2 Se1 Cl2 180.0 2_556 .
Se1 Cl1 Se2 97.21(4) . .
Se1 Cl2 Se2 96.14(4) . .
Cl5 Se2 Cl4 97.34(8) . .
Cl5 Se2 Cl1 93.63(6) . .
Cl4 Se2 Cl1 168.20(6) . .
Cl5 Se2 Cl2 158.15(6) . .
Cl4 Se2 Cl2 101.62(6) . .
Cl1 Se2 Cl2 68.54(4) . .
Se2 Cl4 Se3 78.35(17) . .
Se3 Cl5 Se2 85.8(2) . .
Cl5 Se3 Cl4 95.4(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 C2 1.782(5) .
S1 C9 1.788(4) .
S1 C1 1.793(5) .
S2 C3 1.758(6) .
S2 C8 1.776(6) .
S3 C11 1.754(5) .
S3 C15 1.797(5) .
S4 C12 1.766(5) .
S4 C16 1.796(5) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 C7 1.382(7) .
C2 C3 1.411(7) .
C3 C4 1.391(7) .
C4 C5 1.376(8) .
C4 H4 0.9500 .
C5 C6 1.379(8) .
C5 H5 0.9500 .
C6 C7 1.367(7) .
C6 H6 0.9500 .
C7 H7 0.9500 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 C14 1.389(6) .
C9 C10 1.395(6) .
C10 C11 1.390(6) .
C10 H10 0.9500 .
C11 C12 1.431(6) .
C12 C13 1.383(6) .
C13 C14 1.380(6) .
C13 H13 0.9500 .
C14 H14 0.9500 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
Se1 Cl3 2.3884(13) 2_556
Se1 Cl3 2.3884(13) .
Se1 Cl1 2.4145(14) 2_556
Se1 Cl1 2.4145(14) .
Se1 Cl2 2.4203(13) 2_556
Se1 Cl2 2.4203(13) .
Cl1 Se2 3.0117(17) .
Cl2 Se2 3.0481(16) .
Se2 Cl5 2.1554(19) .
Se2 Cl4 2.209(2) .
Cl4 Se3 2.347(7) .
Cl5 Se3 2.075(7) .
