 
data_TMA-(C2F5SO2)2N at 273K
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             TMA-(C2F5SO2)2N
_chemical_formula_moiety          C8 H12 F10 N2 O4 S2
_chemical_formula_sum 
 'C8 H12 F10 N2 O4 S2' 
_chemical_formula_weight          454.31 
 
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' 
 
_symmetry_cell_setting            'Monoclinic'
_symmetry_space_group_name_H-M    'P21/n'
 
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' 
 
_cell_length_a                    10.1328(8) 
_cell_length_b                    17.3243(14) 
_cell_length_c                    10.2870(8) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  105.3600(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      1741.3(2) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     273(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        'elongate plate'
_exptl_crystal_colour             'colorless'
_exptl_crystal_size_max           0.90
_exptl_crystal_size_mid           0.20
_exptl_crystal_size_min           0.05
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.733 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              912 
_exptl_absorpt_coefficient_mu     0.424 
_exptl_absorpt_correction_type    numerical
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       273(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'sealed tube'
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Bruker APEXII CCD area detector'
_diffrn_measurement_method        'phi and omega scans'
_diffrn_detector_area_resol_mean  8.333
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             10255 
_diffrn_reflns_av_R_equivalents   0.0182 
_diffrn_reflns_av_sigmaI/netI     0.0233 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -22 
_diffrn_reflns_limit_k_max        23 
_diffrn_reflns_limit_l_min        -13 
_diffrn_reflns_limit_l_max        13 
_diffrn_reflns_theta_min          2.37 
_diffrn_reflns_theta_max          28.91 
_reflns_number_total              4208 
_reflns_number_gt                 3001 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'APEX2 '
_computing_cell_refinement        'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction         'SAINT (Bruker AXS, 2004)'
_computing_structure_solution     SIR 2004' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   'ORTEP-III (Farrugia, 1997)'
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0818P)²+1.0806P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          4208 
_refine_ls_number_parameters      239 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0771 
_refine_ls_R_factor_gt            0.0556 
_refine_ls_wR_factor_ref          0.1658 
_refine_ls_wR_factor_gt           0.1475 
_refine_ls_goodness_of_fit_ref    1.030 
_refine_ls_restrained_S_all       1.030 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 
 
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_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
C1 C 0.7582(4) 0.4604(2) -0.0621(4) 0.0737(9) Uani 1 d . . . 
H1A H 0.7702 0.5064 -0.0081 0.111 Uiso 1 calc R . . 
H1B H 0.6792 0.4660 -0.1373 0.111 Uiso 1 calc R . . 
H1C H 0.8378 0.4522 -0.0944 0.111 Uiso 1 calc R . . 
C2 C 0.7159(4) 0.32257(19) -0.0642(3) 0.0691(9) Uani 1 d . . . 
H2A H 0.6369 0.3296 -0.1389 0.104 Uiso 1 calc R . . 
H2B H 0.7015 0.2794 -0.0111 0.104 Uiso 1 calc R . . 
H2C H 0.7946 0.3130 -0.0972 0.104 Uiso 1 calc R . . 
C3 C 0.6178(3) 0.4067(2) 0.0736(3) 0.0672(8) Uani 1 d . . . 
H3A H 0.5377 0.4129 -0.0003 0.101 Uiso 1 calc R . . 
H3B H 0.6317 0.4525 0.1281 0.101 Uiso 1 calc R . . 
H3C H 0.6056 0.3633 0.1273 0.101 Uiso 1 calc R . . 
C4 C 0.8632(3) 0.3834(2) 0.1355(3) 0.0710(9) Uani 1 d . . . 
H4A H 0.9410 0.3734 0.1013 0.107 Uiso 1 calc R . . 
H4B H 0.8498 0.3407 0.1901 0.107 Uiso 1 calc R . . 
H4C H 0.8788 0.4295 0.1890 0.107 Uiso 1 calc R . . 
N1 N 0.7390(2) 0.39341(12) 0.0206(2) 0.0461(5) Uani 1 d . . . 
C11 C 0.7019(3) 0.0684(2) 0.0438(3) 0.0631(8) Uani 1 d . . . 
C12 C 0.7497(5) 0.0645(3) -0.0842(4) 0.0934(13) Uani 1 d . . . 
C13 C 0.7596(3) 0.2233(2) 0.4721(3) 0.0587(7) Uani 1 d . . . 
C14 C 0.6965(5) 0.2924(3) 0.5254(5) 0.0936(13) Uani 1 d . . . 
N11 N 0.7419(3) 0.10579(13) 0.3018(2) 0.0532(6) Uani 1 d . . . 
O11 O 0.9335(2) 0.05833(14) 0.2259(2) 0.0694(6) Uani 1 d . . . 
O12 O 0.8485(2) 0.18685(13) 0.1513(2) 0.0661(6) Uani 1 d . . . 
O13 O 0.5987(2) 0.22699(14) 0.2282(2) 0.0690(6) Uani 1 d . . . 
O14 O 0.5473(2) 0.13487(18) 0.3896(3) 0.0851(8) Uani 1 d . . . 
F11 F 0.6743(3) -0.00409(15) 0.0755(3) 0.1072(9) Uani 1 d . . . 
F12 F 0.5853(2) 0.10821(17) 0.0153(3) 0.1135(10) Uani 1 d . . . 
F13 F 0.6558(3) 0.0296(2) -0.1798(3) 0.1426(13) Uani 1 d . . . 
F14 F 0.8604(3) 0.0264(3) -0.0672(3) 0.1525(15) Uani 1 d . . . 
F15 F 0.7634(6) 0.1333(3) -0.1274(3) 0.186(2) Uani 1 d . . . 
F16 F 0.8672(2) 0.24877(15) 0.4340(2) 0.0910(7) Uani 1 d . . . 
F17 F 0.8071(3) 0.17514(15) 0.5747(2) 0.0973(8) Uani 1 d . . . 
F18 F 0.7824(3) 0.32687(17) 0.6234(3) 0.1178(10) Uani 1 d . . . 
F19 F 0.5934(4) 0.2707(3) 0.5652(5) 0.209(2) Uani 1 d . . . 
F20 F 0.6575(5) 0.3433(2) 0.4294(4) 0.186(2) Uani 1 d . . . 
S11 S 0.82224(7) 0.11161(4) 0.19125(6) 0.0471(2) Uani 1 d . . . 
S12 S 0.64422(7) 0.17071(5) 0.33126(7) 0.0536(2) Uani 1 d . . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
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 
C1 N1 1.482(4) . ? 
C2 N1 1.488(4) . ? 
C3 N1 1.488(4) . ? 
C4 N1 1.491(4) . ? 
C11 F12 1.331(4) . ? 
C11 F11 1.345(4) . ? 
C11 C12 1.521(6) . ? 
C11 S11 1.835(3) . ? 
C12 F14 1.273(5) . ? 
C12 F15 1.291(6) . ? 
C12 F13 1.320(5) . ? 
C13 F16 1.328(3) . ? 
C13 F17 1.331(4) . ? 
C13 C14 1.527(5) . ? 
C13 S12 1.843(3) . ? 
C14 F19 1.276(6) . ? 
C14 F18 1.290(5) . ? 
C14 F20 1.305(6) . ? 
N11 S11 1.568(2) . ? 
N11 S12 1.580(2) . ? 
O11 S11 1.427(2) . ? 
O12 S11 1.413(2) . ? 
O13 S12 1.424(2) . ? 
O14 S12 1.422(2) . ? 
 
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 
C1 N1 C2 109.5(3) . . ? 
C1 N1 C3 109.6(2) . . ? 
C2 N1 C3 109.0(2) . . ? 
C1 N1 C4 109.5(3) . . ? 
C2 N1 C4 109.7(2) . . ? 
C3 N1 C4 109.5(2) . . ? 
F12 C11 F11 107.9(3) . . ? 
F12 C11 C12 107.4(3) . . ? 
F11 C11 C12 107.6(3) . . ? 
F12 C11 S11 109.1(2) . . ? 
F11 C11 S11 108.4(2) . . ? 
C12 C11 S11 116.1(3) . . ? 
F14 C12 F15 110.8(6) . . ? 
F14 C12 F13 107.4(4) . . ? 
F15 C12 F13 106.8(4) . . ? 
F14 C12 C11 112.0(4) . . ? 
F15 C12 C11 110.2(4) . . ? 
F13 C12 C11 109.5(4) . . ? 
F16 C13 F17 106.8(3) . . ? 
F16 C13 C14 107.4(3) . . ? 
F17 C13 C14 107.7(3) . . ? 
F16 C13 S12 109.36(19) . . ? 
F17 C13 S12 109.6(2) . . ? 
C14 C13 S12 115.6(2) . . ? 
F19 C14 F18 109.0(4) . . ? 
F19 C14 F20 109.4(5) . . ? 
F18 C14 F20 106.6(4) . . ? 
F19 C14 C13 109.9(4) . . ? 
F18 C14 C13 112.6(3) . . ? 
F20 C14 C13 109.3(4) . . ? 
S11 N11 S12 124.44(15) . . ? 
O12 S11 O11 118.17(15) . . ? 
O12 S11 N11 116.38(13) . . ? 
O11 S11 N11 107.74(14) . . ? 
O12 S11 C11 105.72(15) . . ? 
O11 S11 C11 104.53(14) . . ? 
N11 S11 C11 102.37(15) . . ? 
O14 S12 O13 119.31(16) . . ? 
O14 S12 N11 107.93(16) . . ? 
O13 S12 N11 116.16(13) . . ? 
O14 S12 C13 104.40(15) . . ? 
O13 S12 C13 105.06(15) . . ? 
N11 S12 C13 101.72(14) . . ? 
 
_diffrn_measured_fraction_theta_max    0.890 
_diffrn_reflns_theta_full              28.91 
_diffrn_measured_fraction_theta_full   0.890 
_refine_diff_density_max    0.444 
_refine_diff_density_min   -0.463 
_refine_diff_density_rms    0.077 
