 
data_s92 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C10 H10 Fe I3' 
_chemical_formula_weight          566.73 
 
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' 
 'Fe'  'Fe'   0.3463   0.8444 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'I'  'I'  -0.4742   1.8119 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            Trigonal 
_symmetry_space_group_name_H-M    R-3 
_symmetry_space_group_name_hall   '-R 3'
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-y, x-y, z' 
 '-x+y, -x, z' 
 'x+2/3, y+1/3, z+1/3' 
 '-y+2/3, x-y+1/3, z+1/3' 
 '-x+y+2/3, -x+1/3, z+1/3' 
 'x+1/3, y+2/3, z+2/3' 
 '-y+1/3, x-y+2/3, z+2/3' 
 '-x+y+1/3, -x+2/3, z+2/3' 
 '-x, -y, -z' 
 'y, -x+y, -z' 
 'x-y, x, -z' 
 '-x+2/3, -y+1/3, -z+1/3' 
 'y+2/3, -x+y+1/3, -z+1/3' 
 'x-y+2/3, x+1/3, -z+1/3' 
 '-x+1/3, -y+2/3, -z+2/3' 
 'y+1/3, -x+y+2/3, -z+2/3' 
 'x-y+1/3, x+2/3, -z+2/3' 
 
 
_cell_length_a                    8.4610(6) 
_cell_length_b                    8.4610(6) 
_cell_length_c                    16.9880(6) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 120.00 
_cell_volume                      1053.21(11) 
_cell_formula_units_Z             3 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     2535 
_cell_measurement_theta_min       2.91 
_cell_measurement_theta_max       27.48 
 
_exptl_crystal_description        Plate 
_exptl_crystal_colour             brown 
_exptl_crystal_size_max           0.20 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.05 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     2.681 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              765 
_exptl_absorpt_coefficient_mu     7.634 
_exptl_absorpt_correction_type    Empirical 
_exptl_absorpt_correction_T_min   0.3105 
_exptl_absorpt_correction_T_max   0.7014 
_exptl_absorpt_process_details    'SORTAV (R. H. Blessing, 1995, 1997)'
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       150(2) 
_diffrn_radiation_wavelength      0.71069 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'Enraf Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Enraf Nonius KappaCCD area detector'
_diffrn_measurement_method        'ω and φ scans to fill Ewald sphere'
_diffrn_detector_area_resol_mean  '9.091 pixels/mm'
_diffrn_standards_number          'n/a'
_diffrn_standards_interval_count  'n/a'
_diffrn_standards_interval_time   'n/a'
_diffrn_standards_decay_%         'n/a'
_diffrn_reflns_number             1416 
_diffrn_reflns_av_R_equivalents   0.1701 
_diffrn_reflns_av_sigmaI/netI     0.1160 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        -10 
_diffrn_reflns_limit_k_max        10 
_diffrn_reflns_limit_l_min        -16 
_diffrn_reflns_limit_l_max        20 
_diffrn_reflns_theta_min          3.03 
_diffrn_reflns_theta_max          26.00 
_reflns_number_total              446 
_reflns_number_gt                 419 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        
;
'DENZO (Otwinowski and Minor, 1997) & COLLECT (Hooft, 1998) '
;
_computing_cell_refinement        'DENZO and COLLECT'
_computing_data_reduction         'DENZO and COLLECT'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_computing_molecular_graphics     ?
_computing_publication_material   SHELXL-97
 
_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)+(0.1023P)²+0.0000P] 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      SHELXL 
_refine_ls_extinction_coef        0.0049(13) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          446 
_refine_ls_number_parameters      28 
_refine_ls_number_restraints      2 
_refine_ls_R_factor_all           0.0613 
_refine_ls_R_factor_gt            0.0600 
_refine_ls_wR_factor_ref          0.1516 
_refine_ls_wR_factor_gt           0.1485 
_refine_ls_goodness_of_fit_ref    1.022 
_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_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
I1 I 0.0000 0.0000 0.5000 0.0263(6) Uani 1 6 d S . . 
I2 I 0.0000 0.0000 0.67260(5) 0.0355(6) Uani 1 3 d S . . 
Fe1 Fe 0.3333 -0.3333 0.6667 0.0324(8) Uani 1 6 d S . . 
C1 C 0.3327(16) -0.1780(15) 0.5677(7) 0.072(3) Uani 1 1 d D . . 
H1 H 0.3323 -0.0660 0.5656 0.086 Uiso 1 1 calc R . . 
C2 C 0.4925(13) -0.1737(14) 0.5692(7) 0.074(3) Uani 1 1 d D . . 
H2 H 0.6045 -0.0613 0.5712 0.089 Uiso 1 1 calc R . . 
 
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 
I1 0.0214(7) 0.0214(7) 0.0361(9) 0.000 0.000 0.0107(3) 
I2 0.0373(7) 0.0373(7) 0.0319(8) 0.000 0.000 0.0187(3) 
Fe1 0.0414(10) 0.0414(10) 0.0144(11) 0.000 0.000 0.0207(5) 
C1 0.076(7) 0.110(10) 0.038(5) 0.027(5) 0.003(4) 0.053(7) 
C2 0.092(8) 0.099(9) 0.054(6) 0.035(6) 0.032(6) 0.064(7) 
 
_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 
I1 I2 2.9321(8) . ? 
I1 I2 2.9321(8) 10_556 ? 
Fe1 C1 2.135(9) 2_545 ? 
Fe1 C1 2.135(9) . ? 
Fe1 C1 2.135(9) 3_655 ? 
Fe1 C1 2.135(9) 13_546 ? 
Fe1 C1 2.135(9) 14_556 ? 
Fe1 C1 2.135(9) 15_446 ? 
Fe1 C2 2.136(10) 2_545 ? 
Fe1 C2 2.136(10) . ? 
Fe1 C2 2.136(10) 3_655 ? 
Fe1 C2 2.136(10) 14_556 ? 
Fe1 C2 2.136(10) 13_546 ? 
Fe1 C2 2.136(10) 15_446 ? 
C1 C2 1.332(7) 2_545 ? 
C1 C2 1.334(7) . ? 
C1 H1 0.9500 . ? 
C2 C1 1.332(7) 3_655 ? 
C2 H2 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 
I2 I1 I2 180.0 . 10_556 ? 
C1 Fe1 C1 64.6(5) 2_545 . ? 
C1 Fe1 C1 64.6(5) 2_545 3_655 ? 
C1 Fe1 C1 64.6(5) . 3_655 ? 
C1 Fe1 C1 115.4(5) 2_545 13_546 ? 
C1 Fe1 C1 179.999(3) . 13_546 ? 
C1 Fe1 C1 115.4(5) 3_655 13_546 ? 
C1 Fe1 C1 180.0(4) 2_545 14_556 ? 
C1 Fe1 C1 115.4(5) . 14_556 ? 
C1 Fe1 C1 115.4(5) 3_655 14_556 ? 
C1 Fe1 C1 64.6(5) 13_546 14_556 ? 
C1 Fe1 C1 115.4(5) 2_545 15_446 ? 
C1 Fe1 C1 115.4(5) . 15_446 ? 
C1 Fe1 C1 179.999(3) 3_655 15_446 ? 
C1 Fe1 C1 64.6(5) 13_546 15_446 ? 
C1 Fe1 C1 64.6(5) 14_556 15_446 ? 
C1 Fe1 C2 36.4(2) 2_545 2_545 ? 
C1 Fe1 C2 36.36(19) . 2_545 ? 
C1 Fe1 C2 77.2(3) 3_655 2_545 ? 
C1 Fe1 C2 143.6(2) 13_546 2_545 ? 
C1 Fe1 C2 143.6(2) 14_556 2_545 ? 
C1 Fe1 C2 102.8(3) 15_446 2_545 ? 
C1 Fe1 C2 77.2(3) 2_545 . ? 
C1 Fe1 C2 36.4(2) . . ? 
C1 Fe1 C2 36.36(19) 3_655 . ? 
C1 Fe1 C2 143.6(2) 13_546 . ? 
C1 Fe1 C2 102.8(3) 14_556 . ? 
C1 Fe1 C2 143.64(19) 15_446 . ? 
C2 Fe1 C2 66.3(5) 2_545 . ? 
C1 Fe1 C2 36.36(19) 2_545 3_655 ? 
C1 Fe1 C2 77.2(3) . 3_655 ? 
C1 Fe1 C2 36.4(2) 3_655 3_655 ? 
C1 Fe1 C2 102.8(3) 13_546 3_655 ? 
C1 Fe1 C2 143.65(19) 14_556 3_655 ? 
C1 Fe1 C2 143.6(2) 15_446 3_655 ? 
C2 Fe1 C2 66.3(5) 2_545 3_655 ? 
C2 Fe1 C2 66.3(5) . 3_655 ? 
C1 Fe1 C2 143.6(2) 2_545 14_556 ? 
C1 Fe1 C2 143.6(2) . 14_556 ? 
C1 Fe1 C2 102.8(3) 3_655 14_556 ? 
C1 Fe1 C2 36.36(19) 13_546 14_556 ? 
C1 Fe1 C2 36.4(2) 14_556 14_556 ? 
C1 Fe1 C2 77.2(3) 15_446 14_556 ? 
C2 Fe1 C2 179.999(4) 2_545 14_556 ? 
C2 Fe1 C2 113.7(5) . 14_556 ? 
C2 Fe1 C2 113.7(5) 3_655 14_556 ? 
C1 Fe1 C2 102.8(3) 2_545 13_546 ? 
C1 Fe1 C2 143.6(2) . 13_546 ? 
C1 Fe1 C2 143.65(19) 3_655 13_546 ? 
C1 Fe1 C2 36.4(2) 13_546 13_546 ? 
C1 Fe1 C2 77.2(3) 14_556 13_546 ? 
C1 Fe1 C2 36.36(19) 15_446 13_546 ? 
C2 Fe1 C2 113.7(5) 2_545 13_546 ? 
C2 Fe1 C2 179.999(2) . 13_546 ? 
C2 Fe1 C2 113.7(5) 3_655 13_546 ? 
C2 Fe1 C2 66.3(5) 14_556 13_546 ? 
C1 Fe1 C2 143.64(19) 2_545 15_446 ? 
C1 Fe1 C2 102.8(3) . 15_446 ? 
C1 Fe1 C2 143.6(2) 3_655 15_446 ? 
C1 Fe1 C2 77.2(3) 13_546 15_446 ? 
C1 Fe1 C2 36.36(19) 14_556 15_446 ? 
C1 Fe1 C2 36.4(2) 15_446 15_446 ? 
C2 Fe1 C2 113.7(5) 2_545 15_446 ? 
C2 Fe1 C2 113.7(5) . 15_446 ? 
C2 Fe1 C2 180.0(7) 3_655 15_446 ? 
C2 Fe1 C2 66.3(5) 14_556 15_446 ? 
C2 Fe1 C2 66.3(5) 13_546 15_446 ? 
C2 C1 C2 122.3(11) 2_545 . ? 
C2 C1 Fe1 71.9(7) 2_545 . ? 
C2 C1 Fe1 71.8(7) . . ? 
C2 C1 H1 118.8 2_545 . ? 
C2 C1 H1 118.8 . . ? 
Fe1 C1 H1 130.3 . . ? 
C1 C2 C1 117.6(12) 3_655 . ? 
C1 C2 Fe1 71.8(7) 3_655 . ? 
C1 C2 Fe1 71.8(7) . . ? 
C1 C2 H2 121.2 3_655 . ? 
C1 C2 H2 121.2 . . ? 
Fe1 C2 H2 127.1 . . ? 
 
_diffrn_measured_fraction_theta_max    0.955 
_diffrn_reflns_theta_full              26.00 
_diffrn_measured_fraction_theta_full   0.955 
_refine_diff_density_max    2.267 
_refine_diff_density_min   -1.423 
_refine_diff_density_rms    0.343 
