#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:21:33 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180134 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/32/7103228.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_7103228
loop_
_publ_author_name
'Risto, Maarit'
'Reed, Robert W'
'Robertson, Craig M'
'Oilunkaniemi, Raija'
'Laitinen, Risto S'
'Oakley, Richard T'
_publ_section_title
;
 Self-association of the N-methyl benzotellurodiazolylium cation:
 implications for the generation of super-heavy atom radicals.
;
_journal_issue                   28
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3278
_journal_page_last               3280
_journal_paper_doi               10.1039/b803159b
_journal_year                    2008
_chemical_formula_sum            'C8 H7 F3 N2 O3 S2'
_chemical_formula_weight         300.28
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 99.424(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.495(2)
_cell_length_b                   11.427(4)
_cell_length_c                   16.481(6)
_cell_measurement_reflns_used    2252
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.19
_cell_measurement_theta_min      3.08
_cell_volume                     1206.6(7)
_computing_cell_refinement       'APEX II'
_computing_data_collection       'APEX II'
_computing_data_reduction        'APEX II'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10772
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    0.48
_exptl_absorpt_correction_T_max  0.9546
_exptl_absorpt_correction_T_min  0.8958
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2629
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0631P)²+0.3804P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1180
_reflns_number_gt                2048
_reflns_number_total             2629
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b803159b.txt
_cod_data_source_block           mebn2sotf_0m
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7103228
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -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
S1' S 0.75018(9) 0.16647(5) 0.66104(4) 0.04660(19) Uani 1 1 d . . .
S1 S 0.77132(10) 0.63344(6) 0.31149(4) 0.0531(2) Uani 1 1 d . . .
O3' O 0.8201(3) 0.28022(16) 0.64073(12) 0.0622(5) Uani 1 1 d . . .
O2' O 0.8506(3) 0.1216(2) 0.73866(12) 0.0758(6) Uani 1 1 d . . .
N2 N 0.8277(3) 0.55523(19) 0.39134(12) 0.0521(5) Uani 1 1 d . . .
C2 C 0.6683(4) 0.4814(2) 0.39775(14) 0.0454(5) Uani 1 1 d . . .
C1 C 0.4956(4) 0.49383(19) 0.33308(14) 0.0433(5) Uani 1 1 d . . .
O1' O 0.5291(3) 0.15226(17) 0.64538(14) 0.0707(6) Uani 1 1 d . . .
N1 N 0.5371(3) 0.57696(17) 0.28002(11) 0.0463(5) Uani 1 1 d . . .
C3 C 0.6616(4) 0.3993(2) 0.46109(16) 0.0562(6) Uani 1 1 d . . .
H3A H 0.7745 0.3889 0.5031 0.067 Uiso 1 1 calc R . .
C7 C 0.3998(4) 0.6131(2) 0.20355(16) 0.0595(7) Uani 1 1 d . . .
H7A H 0.2725 0.5690 0.1973 0.089 Uiso 0.50 1 calc PR . .
H7B H 0.4691 0.5988 0.1573 0.089 Uiso 0.50 1 calc PR . .
H7C H 0.3688 0.6950 0.2064 0.089 Uiso 0.50 1 calc PR . .
H7E H 0.4678 0.6729 0.1767 0.089 Uiso 0.50 1 calc PR . .
H7D H 0.2711 0.6430 0.2167 0.089 Uiso 0.50 1 calc PR . .
H7F H 0.3715 0.5469 0.1676 0.089 Uiso 0.50 1 calc PR . .
C5 C 0.3105(5) 0.3508(2) 0.39358(19) 0.0636(7) Uani 1 1 d . . .
H5A H 0.1912 0.3063 0.3946 0.076 Uiso 1 1 calc R . .
C6 C 0.3128(4) 0.4273(2) 0.33058(17) 0.0538(6) Uani 1 1 d . . .
H6A H 0.1999 0.4351 0.2883 0.065 Uiso 1 1 calc R . .
C4 C 0.4842(5) 0.3360(2) 0.45843(18) 0.0615(7) Uani 1 1 d . . .
H4A H 0.4750 0.2817 0.4997 0.074 Uiso 1 1 calc R . .
F3' F 0.7594(4) 0.0966(2) 0.51095(12) 0.1185(9) Uani 1 1 d . . .
F2' F 0.8027(5) -0.03958(18) 0.60013(17) 0.1304(10) Uani 1 1 d . . .
F1' F 1.0487(4) 0.0804(2) 0.59168(16) 0.1180(8) Uani 1 1 d . . .
C1' C 0.8423(5) 0.0717(3) 0.5864(2) 0.0729(8) Uani 1 1 d . . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
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
O1' S1' O2' 114.75(13) . . ?
O1' S1' O3' 114.13(12) . . ?
O2' S1' O3' 114.69(13) . . ?
O1' S1' C1' 104.10(15) . . ?
O2' S1' C1' 103.85(14) . . ?
O3' S1' C1' 103.36(14) . . ?
N2 S1 N1 96.66(11) . . ?
C2 N2 S1 109.94(16) . . ?
N2 C2 C3 126.1(2) . . ?
N2 C2 C1 113.5(2) . . ?
C3 C2 C1 120.3(2) . . ?
N1 C1 C6 128.3(2) . . ?
N1 C1 C2 109.9(2) . . ?
C6 C1 C2 121.8(2) . . ?
C1 N1 C7 126.4(2) . . ?
C1 N1 S1 110.03(15) . . ?
C7 N1 S1 123.56(18) . . ?
C4 C3 C2 117.4(2) . . ?
C6 C5 C4 122.7(3) . . ?
C5 C6 C1 116.1(2) . . ?
C3 C4 C5 121.6(3) . . ?
F3' C1' F2' 108.2(3) . . ?
F3' C1' F1' 107.4(3) . . ?
F2' C1' F1' 106.4(3) . . ?
F3' C1' S1' 112.7(2) . . ?
F2' C1' S1' 111.3(2) . . ?
F1' C1' S1' 110.6(2) . . ?
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
S1' O1' 1.4262(19) . ?
S1' O2' 1.432(2) . ?
S1' O3' 1.4343(19) . ?
S1' C1' 1.812(3) . ?
S1 N2 1.583(2) . ?
S1 N1 1.656(2) . ?
N2 C2 1.353(3) . ?
C2 C3 1.409(3) . ?
C2 C1 1.422(3) . ?
C1 N1 1.348(3) . ?
C1 C6 1.404(3) . ?
N1 C7 1.478(3) . ?
C3 C4 1.355(4) . ?
C5 C6 1.359(4) . ?
C5 C4 1.431(4) . ?
F3' C1' 1.304(4) . ?
F2' C1' 1.324(4) . ?
F1' C1' 1.333(4) . ?
