 

data_04369a 

 

_audit_creation_method            SHELXL-97 

_chemical_name_systematic 

; 

 ? 

; 

_chemical_name_common             04369a 

_chemical_melting_point           ? 

_chemical_formula_moiety          'C22 H10 F18 S6 W2' 

_chemical_formula_sum             'C22 H10 F18 S6 W2' 

_chemical_formula_weight          1176.36 

 

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' 

 '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' 

 'W'  'W'  -0.8490   6.8722 

 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

 

_symmetry_cell_setting            Orthorhombic 

_symmetry_space_group_name_H-M    Pnma 

 

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' 

 

_cell_length_a                    13.2726(13) 

_cell_length_b                    14.0230(14) 

_cell_length_c                    16.4213(16) 

_cell_angle_alpha                 90.00 

_cell_angle_beta                  90.00 

_cell_angle_gamma                 90.00 

_cell_volume                      3056.4(5) 

_cell_formula_units_Z             4 

_cell_measurement_temperature     173(2) 

_cell_measurement_reflns_used     1955

_cell_measurement_theta_min       2.45

_cell_measurement_theta_max       23.89



_exptl_crystal_description        Needle 

_exptl_crystal_colour             Red 

_exptl_crystal_size_max           0.45 

_exptl_crystal_size_mid           0.03 

_exptl_crystal_size_min           0.02 

_exptl_crystal_density_meas       ? 

_exptl_crystal_density_diffrn     2.556 

_exptl_crystal_density_method     'not measured' 

_exptl_crystal_F_000              2192 

_exptl_absorpt_coefficient_mu     8.059 

_exptl_absorpt_correction_type    Multi-scan 

_exptl_absorpt_correction_T_min   0.1222 

_exptl_absorpt_correction_T_max   0.8554 

_exptl_absorpt_process_details    'SADABS (Sheldrick, 2003)' 

 

_exptl_special_details            'Prof. G. Miessler - St. Olaf' 

 

_diffrn_ambient_temperature       173(2) 

_diffrn_radiation_wavelength      0.71073 

_diffrn_radiation_type            MoK\a 

_diffrn_radiation_source         'sealed tube'

_diffrn_radiation_monochromator  'graphite'

_diffrn_measurement_device_type  'CCD area detector'

_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean  ? 

_diffrn_standards_number          ? 

_diffrn_standards_interval_count  ? 

_diffrn_standards_interval_time   ? 

_diffrn_standards_decay_%         ? 

_diffrn_reflns_number             22888 

_diffrn_reflns_av_R_equivalents   0.1237 

_diffrn_reflns_av_sigmaI/netI     0.0670 

_diffrn_reflns_limit_h_min        0 

_diffrn_reflns_limit_h_max        15 

_diffrn_reflns_limit_k_min        0 

_diffrn_reflns_limit_k_max        16 

_diffrn_reflns_limit_l_min        0 

_diffrn_reflns_limit_l_max        19 

_diffrn_reflns_theta_min          1.91 

_diffrn_reflns_theta_max          25.05 

_reflns_number_total              2824 

_reflns_number_gt                 1988 

_reflns_threshold_expression      >2sigma(I) 

 

_computing_data_collection      'Bruker SMART'

_computing_cell_refinement      'Bruker SMART'

_computing_data_reduction       'Bruker SAINT'

_computing_structure_solution   'Bruker SHELXTL'

_computing_structure_refinement 'Bruker SHELXTL'

_computing_molecular_graphics   'Bruker SHELXTL'

_computing_publication_material 'Bruker SHELXTL'

 

_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)+(0.0207P)²+65.6472P] 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          2824 

_refine_ls_number_parameters      217 

_refine_ls_number_restraints      138 

_refine_ls_R_factor_all           0.0889 

_refine_ls_R_factor_gt            0.0469 

_refine_ls_wR_factor_ref          0.1052 

_refine_ls_wR_factor_gt           0.0888 

_refine_ls_goodness_of_fit_ref    1.067 

_refine_ls_restrained_S_all       1.084 

_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_symmetry_multiplicity 

 _atom_site_calc_flag 

 _atom_site_refinement_flags 

 _atom_site_disorder_assembly 

 _atom_site_disorder_group 

W1 W 0.32471(5) 0.2500 0.78733(4) 0.0228(2) Uani 1 2 d S . . 

W2 W 0.34958(5) 0.2500 0.57018(4) 0.0244(2) Uani 1 2 d S . . 

S1 S 0.1918(2) 0.1391(2) 0.7928(2) 0.0307(7) Uani 1 1 d . . . 

S2 S 0.3843(2) 0.1417(2) 0.68669(19) 0.0256(7) Uani 1 1 d . . . 

S3 S 0.2241(2) 0.1413(2) 0.5366(2) 0.0298(8) Uani 1 1 d . A . 

C1 C 0.1607(6) -0.0445(6) 0.7549(5) 0.047(4) Uani 1 1 d D . . 

F1 F 0.1307(8) -0.0524(7) 0.8318(5) 0.116(5) Uani 1 1 d D . . 

F2 F 0.1966(7) -0.1301(6) 0.7359(7) 0.107(4) Uani 1 1 d D . . 

F3 F 0.0760(6) -0.0365(6) 0.7124(6) 0.083(3) Uani 1 1 d D . . 

C2 C 0.2299(9) 0.0367(9) 0.7404(8) 0.034(3) Uani 1 1 d . . . 

C3 C 0.3084(9) 0.0365(9) 0.6911(7) 0.031(3) Uani 1 1 d . . . 

C4 C 0.3442(5) -0.0434(6) 0.6386(5) 0.043(4) Uani 1 1 d D . . 

F4 F 0.2723(6) -0.0856(6) 0.5954(5) 0.075(3) Uani 1 1 d D . . 

F5 F 0.3884(6) -0.1135(5) 0.6798(5) 0.057(2) Uani 1 1 d D . . 

F6 F 0.4123(6) -0.0159(5) 0.5841(5) 0.066(3) Uani 1 1 d D . . 

C5 C 0.0734(6) 0.1405(6) 0.4244(5) 0.046(4) Uani 0.50 1 d PD A 1 

F7 F 0.0566(11) 0.0602(8) 0.4658(8) 0.059(3) Uiso 0.50 1 d PD A 1 

F8 F 0.1048(9) 0.1116(10) 0.3518(6) 0.050(3) Uiso 0.50 1 d PD A 1 

F9 F -0.0186(7) 0.1756(10) 0.4124(8) 0.044(3) Uiso 0.50 1 d PD A 1 

C5' C 0.0734(6) 0.1405(6) 0.4244(5) 0.046(4) Uani 0.50 1 d PD A 2 

F7' F 0.1110(9) 0.0547(7) 0.4085(9) 0.044(3) Uiso 0.50 1 d PD A 2 

F8' F 0.0692(10) 0.1827(10) 0.3517(7) 0.059(3) Uiso 0.50 1 d PD A 2 

F9' F -0.0222(6) 0.1262(10) 0.4446(8) 0.050(3) Uiso 0.50 1 d PD A 2 

C6 C 0.1390(8) 0.2020(9) 0.4749(7) 0.029(3) Uani 1 1 d . . . 

C7 C 0.3521(12) 0.2021(16) 0.9202(10) 0.111(12) Uani 1 1 d D . . 

H7A H 0.3054 0.1629 0.9485 0.133 Uiso 1 1 calc R . . 

C8 C 0.4313(11) 0.1693(10) 0.8725(9) 0.068(6) Uani 1 1 d D . . 

H8A H 0.4480 0.1047 0.8613 0.081 Uiso 1 1 calc R . . 

C9 C 0.4809(13) 0.2500 0.8444(11) 0.043(6) Uani 1 2 d SD . . 

H9A H 0.5396 0.2500 0.8113 0.052 Uiso 1 2 calc SR . . 

C10 C 0.5152(9) 0.1998(11) 0.5358(8) 0.053(5) Uani 1 1 d D . . 

H10A H 0.5555 0.1597 0.5692 0.064 Uiso 1 1 calc R . . 

C11 C 0.4455(8) 0.1702(11) 0.4780(7) 0.048(4) Uani 1 1 d D . . 

H11A H 0.4298 0.1058 0.4652 0.058 Uiso 1 1 calc R . . 

C12 C 0.4023(12) 0.2500 0.4420(11) 0.038(5) Uani 1 2 d SD . . 

H12A H 0.3526 0.2500 0.4004 0.045 Uiso 1 2 calc SR . . 

 


 

_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 

W1 C9 2.275(17) . ? 

W1 C8 2.288(13) . ? 

W1 C8 2.288(13) 7_565 ? 

W1 C7 2.312(17) 7_565 ? 

W1 C7 2.312(17) . ? 

W1 S1 2.353(3) 7_565 ? 

W1 S1 2.353(3) . ? 

W1 S2 2.380(3) 7_565 ? 

W1 S2 2.380(3) . ? 

W2 C12 2.218(17) . ? 

W2 C11 2.272(13) . ? 

W2 C11 2.272(13) 7_565 ? 

W2 S3 2.324(3) . ? 

W2 S3 2.324(3) 7_565 ? 

W2 C10 2.376(12) . ? 

W2 C10 2.376(12) 7_565 ? 

W2 S2 2.486(3) . ? 

W2 S2 2.486(3) 7_565 ? 

S1 C2 1.748(14) . ? 

S2 C3 1.787(13) . ? 

S3 C6 1.740(12) . ? 

C1 F2 1.329(5) . ? 

C1 F3 1.329(5) . ? 

C1 F1 1.329(5) . ? 

C1 C2 1.482(16) . ? 

C2 C3 1.320(17) . ? 

C3 C4 1.492(16) . ? 

C4 F4 1.329(5) . ? 

C4 F5 1.329(5) . ? 

C4 F6 1.330(5) . ? 

C5 F8 1.326(5) . ? 

C5 F9 1.331(5) . ? 

C5 F7 1.334(5) . ? 

C5 C6 1.479(15) . ? 

C6 C6 1.35(3) 7_565 ? 

C7 C7 1.34(4) 7_565 ? 

C7 C8 1.389(10) . ? 

C7 H7A 0.9500 . ? 

C8 C9 1.389(10) . ? 

C8 H8A 0.9500 . ? 

C9 C8 1.389(10) 7_565 ? 

C9 H9A 0.9500 . ? 

C10 C11 1.389(10) . ? 

C10 C10 1.41(3) 7_565 ? 

C10 H10A 0.9500 . ? 

C11 C12 1.389(10) . ? 

C11 H11A 0.9500 . ? 

C12 C11 1.389(10) 7_565 ? 

C12 H12A 0.9500 . ? 

 

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 

C9 W1 C8 35.4(3) . . ? 

C9 W1 C8 35.4(3) . 7_565 ? 

C8 W1 C8 59.3(7) . 7_565 ? 

C9 W1 C7 57.8(6) . 7_565 ? 

C8 W1 C7 58.0(6) . 7_565 ? 

C8 W1 C7 35.1(3) 7_565 7_565 ? 

C9 W1 C7 57.8(6) . . ? 

C8 W1 C7 35.1(3) . . ? 

C8 W1 C7 58.0(6) 7_565 . ? 

C7 W1 C7 33.8(11) 7_565 . ? 

C9 W1 S1 131.8(2) . 7_565 ? 

C8 W1 S1 140.1(4) . 7_565 ? 

C8 W1 S1 96.5(3) 7_565 7_565 ? 

C7 W1 S1 83.7(4) 7_565 7_565 ? 

C7 W1 S1 105.9(5) . 7_565 ? 

C9 W1 S1 131.8(2) . . ? 

C8 W1 S1 96.5(3) . . ? 

C8 W1 S1 140.1(4) 7_565 . ? 

C7 W1 S1 105.9(5) 7_565 . ? 

C7 W1 S1 83.7(4) . . ? 

S1 W1 S1 82.75(16) 7_565 . ? 

C9 W1 S2 89.0(4) . 7_565 ? 

C8 W1 S2 122.3(4) . 7_565 ? 

C8 W1 S2 84.4(4) 7_565 7_565 ? 

C7 W1 S2 114.7(6) 7_565 7_565 ? 

C7 W1 S2 142.0(4) . 7_565 ? 

S1 W1 S2 81.60(11) 7_565 7_565 ? 

S1 W1 S2 134.24(11) . 7_565 ? 

C9 W1 S2 89.0(4) . . ? 

C8 W1 S2 84.4(4) . . ? 

C8 W1 S2 122.3(4) 7_565 . ? 

C7 W1 S2 142.0(4) 7_565 . ? 

C7 W1 S2 114.7(6) . . ? 

S1 W1 S2 134.24(11) 7_565 . ? 

S1 W1 S2 81.60(11) . . ? 

S2 W1 S2 79.32(16) 7_565 . ? 

C12 W2 C11 36.0(2) . . ? 

C12 W2 C11 36.0(2) . 7_565 ? 

C11 W2 C11 59.0(7) . 7_565 ? 

C12 W2 S3 90.1(3) . . ? 

C11 W2 S3 85.4(4) . . ? 

C11 W2 S3 124.5(3) 7_565 . ? 

C12 W2 S3 90.1(3) . 7_565 ? 

C11 W2 S3 124.5(3) . 7_565 ? 

C11 W2 S3 85.4(4) 7_565 7_565 ? 

S3 W2 S3 81.99(16) . 7_565 ? 

C12 W2 C10 58.8(5) . . ? 

C11 W2 C10 34.7(2) . . ? 

C11 W2 C10 58.0(5) 7_565 . ? 

S3 W2 C10 114.4(4) . . ? 

S3 W2 C10 143.2(4) 7_565 . ? 

C12 W2 C10 58.8(5) . 7_565 ? 

C11 W2 C10 58.0(5) . 7_565 ? 

C11 W2 C10 34.7(2) 7_565 7_565 ? 

S3 W2 C10 143.2(4) . 7_565 ? 

S3 W2 C10 114.4(4) 7_565 7_565 ? 

C10 W2 C10 34.5(8) . 7_565 ? 

C12 W2 S2 132.2(3) . . ? 

C11 W2 S2 96.2(3) . . ? 

C11 W2 S2 135.2(3) 7_565 . ? 

S3 W2 S2 85.09(11) . . ? 

S3 W2 S2 135.73(11) 7_565 . ? 

C10 W2 S2 80.2(4) . . ? 

C10 W2 S2 101.1(3) 7_565 . ? 

C12 W2 S2 132.2(3) . 7_565 ? 

C11 W2 S2 135.2(3) . 7_565 ? 

C11 W2 S2 96.2(3) 7_565 7_565 ? 

S3 W2 S2 135.73(11) . 7_565 ? 

S3 W2 S2 85.09(11) 7_565 7_565 ? 

C10 W2 S2 101.1(3) . 7_565 ? 

C10 W2 S2 80.2(4) 7_565 7_565 ? 

S2 W2 S2 75.33(15) . 7_565 ? 

C2 S1 W1 107.9(4) . . ? 

C3 S2 W1 108.1(4) . . ? 

C3 S2 W2 115.5(4) . . ? 

W1 S2 W2 94.75(11) . . ? 

C6 S3 W2 106.4(4) . . ? 

F2 C1 F3 104.8(5) . . ? 

F2 C1 F1 104.8(5) . . ? 

F3 C1 F1 104.6(5) . . ? 

F2 C1 C2 115.8(8) . . ? 

F3 C1 C2 112.0(8) . . ? 

F1 C1 C2 113.8(9) . . ? 

C3 C2 C1 125.9(12) . . ? 

C3 C2 S1 122.1(11) . . ? 

C1 C2 S1 111.9(9) . . ? 

C2 C3 C4 127.4(11) . . ? 

C2 C3 S2 117.9(10) . . ? 

C4 C3 S2 114.6(8) . . ? 

F4 C4 F5 105.0(5) . . ? 

F4 C4 F6 104.9(5) . . ? 

F5 C4 F6 104.9(5) . . ? 

F4 C4 C3 114.5(8) . . ? 

F5 C4 C3 113.8(8) . . ? 

F6 C4 C3 112.8(8) . . ? 

F8 C5 F9 105.5(5) . . ? 

F8 C5 F7 104.6(5) . . ? 

F9 C5 F7 103.6(5) . . ? 

F8 C5 C6 119.7(9) . . ? 

F9 C5 C6 114.1(9) . . ? 

F7 C5 C6 107.7(10) . . ? 

C6 C6 C5 125.6(6) 7_565 . ? 

C6 C6 S3 119.3(4) 7_565 . ? 

C5 C6 S3 115.1(8) . . ? 

C7 C7 C8 109.3(10) 7_565 . ? 

C7 C7 W1 73.1(5) 7_565 . ? 

C8 C7 W1 71.5(9) . . ? 

C7 C7 H7A 125.3 7_565 . ? 

C8 C7 H7A 125.3 . . ? 

W1 C7 H7A 121.7 . . ? 

C9 C8 C7 106.0(14) . . ? 

C9 C8 W1 71.8(9) . . ? 

C7 C8 W1 73.4(10) . . ? 

C9 C8 H8A 127.0 . . ? 

C7 C8 H8A 127.0 . . ? 

W1 C8 H8A 119.8 . . ? 

C8 C9 C8 109.2(17) 7_565 . ? 

C8 C9 W1 72.8(9) 7_565 . ? 

C8 C9 W1 72.8(9) . . ? 

C8 C9 H9A 125.4 7_565 . ? 

C8 C9 H9A 125.4 . . ? 

W1 C9 H9A 120.7 . . ? 

C11 C10 C10 107.4(9) . 7_565 ? 

C11 C10 W2 68.5(7) . . ? 

C10 C10 W2 72.8(4) 7_565 . ? 

C11 C10 H10A 126.3 . . ? 

C10 C10 H10A 126.3 7_565 . ? 

W2 C10 H10A 124.0 . . ? 

C12 C11 C10 108.9(15) . . ? 

C12 C11 W2 69.9(9) . . ? 

C10 C11 W2 76.8(8) . . ? 

C12 C11 H11A 125.5 . . ? 

C10 C11 H11A 125.5 . . ? 

W2 C11 H11A 119.5 . . ? 

C11 C12 C11 107.3(16) 7_565 . ? 

C11 C12 W2 74.1(9) 7_565 . ? 

C11 C12 W2 74.1(9) . . ? 

C11 C12 H12A 126.3 7_565 . ? 

C11 C12 H12A 126.3 . . ? 

W2 C12 H12A 117.5 . . ? 

 

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 

C9 W1 S1 C2 -68.1(7) . . . . ? 

C8 W1 S1 C2 -70.4(6) . . . . ? 

C8 W1 S1 C2 -118.7(7) 7_565 . . . ? 

C7 W1 S1 C2 -128.9(6) 7_565 . . . ? 

C7 W1 S1 C2 -103.1(7) . . . . ? 

S1 W1 S1 C2 149.9(4) 7_565 . . . ? 

S2 W1 S1 C2 79.1(5) 7_565 . . . ? 

S2 W1 S1 C2 13.0(5) . . . . ? 

C9 W1 S2 C3 121.9(5) . . . . ? 

C8 W1 S2 C3 86.7(5) . . . . ? 

C8 W1 S2 C3 134.8(6) 7_565 . . . ? 

C7 W1 S2 C3 94.4(10) 7_565 . . . ? 

C7 W1 S2 C3 68.3(6) . . . . ? 

S1 W1 S2 C3 -81.9(4) 7_565 . . . ? 

S1 W1 S2 C3 -10.7(4) . . . . ? 

S2 W1 S2 C3 -148.9(4) 7_565 . . . ? 

C9 W1 S2 W2 -119.3(3) . . . . ? 

C8 W1 S2 W2 -154.5(3) . . . . ? 

C8 W1 S2 W2 -106.4(5) 7_565 . . . ? 

C7 W1 S2 W2 -146.8(9) 7_565 . . . ? 

C7 W1 S2 W2 -172.9(4) . . . . ? 

S1 W1 S2 W2 36.89(18) 7_565 . . . ? 

S1 W1 S2 W2 108.12(11) . . . . ? 

S2 W1 S2 W2 -30.08(13) 7_565 . . . ? 

C12 W2 S2 C3 -83.7(7) . . . . ? 

C11 W2 S2 C3 -82.9(6) . . . . ? 

C11 W2 S2 C3 -134.2(6) 7_565 . . . ? 

S3 W2 S2 C3 1.9(5) . . . . ? 

S3 W2 S2 C3 75.1(5) 7_565 . . . ? 

C10 W2 S2 C3 -113.9(6) . . . . ? 

C10 W2 S2 C3 -141.4(6) 7_565 . . . ? 

S2 W2 S2 C3 141.9(5) 7_565 . . . ? 

C12 W2 S2 W1 163.6(5) . . . . ? 

C11 W2 S2 W1 164.4(3) . . . . ? 

C11 W2 S2 W1 113.1(4) 7_565 . . . ? 

S3 W2 S2 W1 -110.77(11) . . . . ? 

S3 W2 S2 W1 -37.54(18) 7_565 . . . ? 

C10 W2 S2 W1 133.5(4) . . . . ? 

C10 W2 S2 W1 105.9(4) 7_565 . . . ? 

S2 W2 S2 W1 29.17(12) 7_565 . . . ? 

C12 W2 S3 C6 -68.7(5) . . . . ? 

C11 W2 S3 C6 -104.4(5) . . . . ? 

C11 W2 S3 C6 -57.4(6) 7_565 . . . ? 

S3 W2 S3 C6 21.4(4) 7_565 . . . ? 

C10 W2 S3 C6 -124.1(6) . . . . ? 

C10 W2 S3 C6 -99.1(7) 7_565 . . . ? 

S2 W2 S3 C6 158.9(4) . . . . ? 

S2 W2 S3 C6 95.8(4) 7_565 . . . ? 

F2 C1 C2 C3 20.4(15) . . . . ? 

F3 C1 C2 C3 -99.8(13) . . . . ? 

F1 C1 C2 C3 141.9(12) . . . . ? 

F2 C1 C2 S1 -162.9(6) . . . . ? 

F3 C1 C2 S1 76.9(9) . . . . ? 

F1 C1 C2 S1 -41.4(10) . . . . ? 

W1 S1 C2 C3 -15.2(12) . . . . ? 

W1 S1 C2 C1 168.0(6) . . . . ? 

C1 C2 C3 C4 1(2) . . . . ? 

S1 C2 C3 C4 -175.4(8) . . . . ? 

C1 C2 C3 S2 -177.4(8) . . . . ? 

S1 C2 C3 S2 6.3(15) . . . . ? 

W1 S2 C3 C2 5.8(11) . . . . ? 

W2 S2 C3 C2 -98.8(10) . . . . ? 

W1 S2 C3 C4 -172.7(6) . . . . ? 

W2 S2 C3 C4 82.6(8) . . . . ? 

C2 C3 C4 F4 47.3(14) . . . . ? 

S2 C3 C4 F4 -134.3(6) . . . . ? 

C2 C3 C4 F5 -73.5(13) . . . . ? 

S2 C3 C4 F5 104.9(8) . . . . ? 

C2 C3 C4 F6 167.1(11) . . . . ? 

S2 C3 C4 F6 -14.5(9) . . . . ? 

F8 C5 C6 C6 91.3(8) . . . 7_565 ? 

F9 C5 C6 C6 -35.1(9) . . . 7_565 ? 

F7 C5 C6 C6 -149.5(6) . . . 7_565 ? 

F8 C5 C6 S3 -87.1(10) . . . . ? 

F9 C5 C6 S3 146.5(8) . . . . ? 

F7 C5 C6 S3 32.1(10) . . . . ? 

W2 S3 C6 C6 -18.4(4) . . . 7_565 ? 

W2 S3 C6 C5 160.2(7) . . . . ? 

C9 W1 C7 C7 79.0(4) . . . 7_565 ? 

C8 W1 C7 C7 117.8(9) . . . 7_565 ? 

C8 W1 C7 C7 36.9(3) 7_565 . . 7_565 ? 

S1 W1 C7 C7 -50.82(17) 7_565 . . 7_565 ? 

S1 W1 C7 C7 -131.40(12) . . . 7_565 ? 

S2 W1 C7 C7 46.0(6) 7_565 . . 7_565 ? 

S2 W1 C7 C7 150.9(3) . . . 7_565 ? 

C9 W1 C7 C8 -38.8(8) . . . . ? 

C8 W1 C7 C8 -80.9(10) 7_565 . . . ? 

C7 W1 C7 C8 -117.8(9) 7_565 . . . ? 

S1 W1 C7 C8 -168.6(8) 7_565 . . . ? 

S1 W1 C7 C8 110.8(10) . . . . ? 

S2 W1 C7 C8 -71.8(14) 7_565 . . . ? 

S2 W1 C7 C8 33.1(10) . . . . ? 

C7 C7 C8 C9 1.1(13) 7_565 . . . ? 

W1 C7 C8 C9 64.8(11) . . . . ? 

C7 C7 C8 W1 -63.7(4) 7_565 . . . ? 

C8 W1 C8 C9 -36.9(9) 7_565 . . . ? 

C7 W1 C8 C9 -78.2(12) 7_565 . . . ? 

C7 W1 C8 C9 -113.7(14) . . . . ? 

S1 W1 C8 C9 -96.5(8) 7_565 . . . ? 

S1 W1 C8 C9 177.0(8) . . . . ? 

S2 W1 C8 C9 22.6(10) 7_565 . . . ? 

S2 W1 C8 C9 96.2(8) . . . . ? 

C9 W1 C8 C7 113.7(14) . . . . ? 

C8 W1 C8 C7 76.8(11) 7_565 . . . ? 

C7 W1 C8 C7 35.5(12) 7_565 . . . ? 

S1 W1 C8 C7 17.2(12) 7_565 . . . ? 

S1 W1 C8 C7 -69.3(10) . . . . ? 

S2 W1 C8 C7 136.3(10) 7_565 . . . ? 

S2 W1 C8 C7 -150.1(10) . . . . ? 

C7 C8 C9 C8 -2(2) . . . 7_565 ? 

W1 C8 C9 C8 64.2(13) . . . 7_565 ? 

C7 C8 C9 W1 -65.9(11) . . . . ? 

C8 W1 C9 C8 -117.2(17) . . . 7_565 ? 

C7 W1 C9 C8 -38.5(8) 7_565 . . 7_565 ? 

C7 W1 C9 C8 -78.7(13) . . . 7_565 ? 

S1 W1 C9 C8 3.9(11) 7_565 . . 7_565 ? 

S1 W1 C9 C8 -121.1(7) . . . 7_565 ? 

S2 W1 C9 C8 81.8(9) 7_565 . . 7_565 ? 

S2 W1 C9 C8 161.1(9) . . . 7_565 ? 

C8 W1 C9 C8 117.2(17) 7_565 . . . ? 

C7 W1 C9 C8 78.7(13) 7_565 . . . ? 

C7 W1 C9 C8 38.5(8) . . . . ? 

S1 W1 C9 C8 121.1(7) 7_565 . . . ? 

S1 W1 C9 C8 -3.9(11) . . . . ? 

S2 W1 C9 C8 -161.1(9) 7_565 . . . ? 

S2 W1 C9 C8 -81.8(9) . . . . ? 

C12 W2 C10 C11 -38.1(8) . . . . ? 

C11 W2 C10 C11 -80.6(10) 7_565 . . . ? 

S3 W2 C10 C11 36.1(9) . . . . ? 

S3 W2 C10 C11 -74.3(11) 7_565 . . . ? 

C10 W2 C10 C11 -117.3(8) 7_565 . . . ? 

S2 W2 C10 C11 116.2(9) . . . . ? 

S2 W2 C10 C11 -171.0(8) 7_565 . . . ? 

C12 W2 C10 C10 79.2(3) . . . 7_565 ? 

C11 W2 C10 C10 117.3(8) . . . 7_565 ? 

C11 W2 C10 C10 36.6(3) 7_565 . . 7_565 ? 

S3 W2 C10 C10 153.4(3) . . . 7_565 ? 

S3 W2 C10 C10 42.9(4) 7_565 . . 7_565 ? 

S2 W2 C10 C10 -126.57(12) . . . 7_565 ? 

S2 W2 C10 C10 -53.77(11) 7_565 . . 7_565 ? 

C10 C10 C11 C12 0.2(12) 7_565 . . . ? 

W2 C10 C11 C12 63.0(10) . . . . ? 

C10 C10 C11 W2 -62.8(4) 7_565 . . . ? 

C11 W2 C11 C12 -38.9(8) 7_565 . . . ? 

S3 W2 C11 C12 96.4(8) . . . . ? 

S3 W2 C11 C12 19.4(10) 7_565 . . . ? 

C10 W2 C11 C12 -116.2(14) . . . . ? 

C10 W2 C11 C12 -79.8(10) 7_565 . . . ? 

S2 W2 C11 C12 -179.0(8) . . . . ? 

S2 W2 C11 C12 -103.6(6) 7_565 . . . ? 

C12 W2 C11 C10 116.2(14) . . . . ? 

C11 W2 C11 C10 77.3(8) 7_565 . . . ? 

S3 W2 C11 C10 -147.4(9) . . . . ? 

S3 W2 C11 C10 135.6(7) 7_565 . . . ? 

C10 W2 C11 C10 36.4(9) 7_565 . . . ? 

S2 W2 C11 C10 -62.8(9) . . . . ? 

S2 W2 C11 C10 12.5(11) 7_565 . . . ? 

C10 C11 C12 C11 -0.2(19) . . . 7_565 ? 

W2 C11 C12 C11 67.2(12) . . . 7_565 ? 

C10 C11 C12 W2 -67.5(9) . . . . ? 

C11 W2 C12 C11 -113.8(15) . . . 7_565 ? 

S3 W2 C12 C11 164.1(8) . . . 7_565 ? 

S3 W2 C12 C11 82.1(8) 7_565 . . 7_565 ? 

C10 W2 C12 C11 -77.1(10) . . . 7_565 ? 

C10 W2 C12 C11 -36.6(8) 7_565 . . 7_565 ? 

S2 W2 C12 C11 -112.5(6) . . . 7_565 ? 

S2 W2 C12 C11 -1.3(10) 7_565 . . 7_565 ? 

C11 W2 C12 C11 113.8(15) 7_565 . . . ? 

S3 W2 C12 C11 -82.1(8) . . . . ? 

S3 W2 C12 C11 -164.1(8) 7_565 . . . ? 

C10 W2 C12 C11 36.7(8) . . . . ? 

C10 W2 C12 C11 77.1(10) 7_565 . . . ? 

S2 W2 C12 C11 1.3(10) . . . . ? 

S2 W2 C12 C11 112.5(6) 7_565 . . . ? 

 

_diffrn_measured_fraction_theta_max    0.999 

_diffrn_reflns_theta_full              25.05 

_diffrn_measured_fraction_theta_full   0.999 

_refine_diff_density_max    2.105 

_refine_diff_density_min   -1.625 

_refine_diff_density_rms    0.262 

