# Copyright The Royal Society of Chemistry, 1999
# CCDC Number: 182/1154 
data_k9850 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C19 H22 B Cl Fe Sn' 
_chemical_formula_weight          471.17 
 
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' 
 'B'  'B'   0.0013   0.0007 
 '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' 
 'Fe'  'Fe'   0.3463   0.8444 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Sn'  'Sn'  -0.6537   1.4246 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            ? 
_symmetry_space_group_name_H-M    ? 
 
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                    11.0509(4) 
_cell_length_b                    14.1655(7) 
_cell_length_c                    11.7913(5) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  95.826(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      1836.3(6) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     150.0(1)
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           ? 
_exptl_crystal_size_mid           ? 
_exptl_crystal_size_min           ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.704 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              936 
_exptl_absorpt_coefficient_mu     2.291 
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    'Scalepack (Otwinowski & Minor, 1997)'
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       150.0(1)
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Nonius KappaCCD'
_diffrn_measurement_method        'phi scans'
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             3145 
_diffrn_reflns_av_R_equivalents   0.0000 
_diffrn_reflns_av_sigmaI/netI     0.0390 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        16 
_diffrn_reflns_limit_l_min        -14 
_diffrn_reflns_limit_l_max        13 
_diffrn_reflns_theta_min          4.19 
_diffrn_reflns_theta_max          25.05 
_reflns_number_total              3145 
_reflns_number_gt                 2688 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'KappaCCD server software (Nonius, 1997)' 
_computing_cell_refinement        'Denzo-SMN (Otwinowski & Minor, 1997)' 
_computing_data_reduction         'Denzo-SMN (Otwinowski & Minor, 1997)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Bruker SHELXTL V5.1' 
_computing_publication_material   'Bruker SHELXTL V5.1' 
 
_refine_special_details 
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ 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/[\s^2^(Fo^2^)+(0.0441P)^2^+1.5093P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.0027(5) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_number_reflns          3145 
_refine_ls_number_parameters      212 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0383 
_refine_ls_R_factor_gt            0.0307 
_refine_ls_wR_factor_ref          0.0825 
_refine_ls_wR_factor_gt           0.0786 
_refine_ls_goodness_of_fit_ref    1.067 
_refine_ls_restrained_S_all       1.067 
_refine_ls_shift/su_max           0.019 
_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 
Sn1 Sn 0.57285(2) 0.051716(18) 1.28851(2) 0.02557(12) Uani 1 1 d . . . 
Fe1 Fe 0.86497(4) 0.08556(4) 1.17113(4) 0.02501(16) Uani 1 1 d . . . 
Cl1 Cl 0.68389(10) -0.02904(8) 1.44544(9) 0.0406(3) Uani 1 1 d . . . 
C1 C 0.6943(3) 0.0273(3) 1.1634(3) 0.0257(8) Uani 1 1 d . . . 
B1 B 0.6617(4) 0.1731(3) 1.0161(3) 0.0289(9) Uani 1 1 d . . . 
C2 C 0.7131(3) 0.0770(3) 1.0578(3) 0.0274(8) Uani 1 1 d . . . 
C3 C 0.8159(3) 0.0316(3) 1.0132(3) 0.0291(8) Uani 1 1 d . . . 
H3A H 0.8516 0.0502 0.9418 0.035 Uiso 1 1 calc R . . 
C4 C 0.8583(3) -0.0424(3) 1.0872(4) 0.0331(9) Uani 1 1 d . . . 
H4A H 0.9292 -0.0844 1.0777 0.040 Uiso 1 1 calc R . . 
C5 C 0.7843(3) -0.0450(3) 1.1790(4) 0.0293(8) Uani 1 1 d . . . 
H5A H 0.7954 -0.0892 1.2454 0.035 Uiso 1 1 calc R . . 
C6 C 0.8867(3) 0.1778(3) 1.3071(3) 0.0370(10) Uani 1 1 d . . . 
H6A H 0.8239 0.1938 1.3594 0.044 Uiso 1 1 calc R . . 
C7 C 0.9060(4) 0.2252(3) 1.2057(4) 0.0374(10) Uani 1 1 d . . . 
H7A H 0.8587 0.2809 1.1732 0.045 Uiso 1 1 calc R . . 
C8 C 1.0025(3) 0.1800(3) 1.1565(4) 0.0365(9) Uani 1 1 d . . . 
H8A H 1.0366 0.1986 1.0844 0.044 Uiso 1 1 calc R . . 
C9 C 1.0431(3) 0.1042(3) 1.2294(3) 0.0353(9) Uani 1 1 d . . . 
H9A H 1.1110 0.0599 1.2173 0.042 Uiso 1 1 calc R . . 
C10 C 0.9721(3) 0.1025(3) 1.3217(3) 0.0352(9) Uani 1 1 d . . . 
H10A H 0.9806 0.0566 1.3865 0.042 Uiso 1 1 calc R . . 
C11 C 0.5426(3) 0.2129(3) 1.0606(3) 0.0260(8) Uani 1 1 d . . . 
C12 C 0.4416(3) 0.1544(3) 1.0658(3) 0.0275(8) Uani 1 1 d . . . 
H12A H 0.4474 0.0895 1.0465 0.033 Uiso 1 1 calc R . . 
C13 C 0.3323(3) 0.1891(3) 1.0985(3) 0.0338(9) Uani 1 1 d . . . 
H13A H 0.2647 0.1480 1.1007 0.041 Uiso 1 1 calc R . . 
C14 C 0.3221(4) 0.2826(3) 1.1278(3) 0.0358(9) Uani 1 1 d . . . 
H14A H 0.2477 0.3062 1.1503 0.043 Uiso 1 1 calc R . . 
C15 C 0.4220(4) 0.3425(3) 1.1240(3) 0.0363(9) Uani 1 1 d . . . 
H15A H 0.4161 0.4068 1.1457 0.044 Uiso 1 1 calc R . . 
C16 C 0.5291(4) 0.3085(3) 1.0889(3) 0.0320(9) Uani 1 1 d . . . 
H16A H 0.5952 0.3507 1.0838 0.038 Uiso 1 1 calc R . . 
C17 C 0.7259(3) 0.2343(2) 0.9224(3) 0.0186(7) Uani 1 1 d . . . 
H17A H 0.8004 0.2024 0.9047 0.028 Uiso 1 1 calc R . . 
H17B H 0.7461 0.2972 0.9531 0.028 Uiso 1 1 calc R . . 
H17C H 0.6699 0.2402 0.8528 0.028 Uiso 1 1 calc R . . 
C18 C 0.4130(4) -0.0330(3) 1.2647(4) 0.0396(10) Uani 1 1 d . . . 
H18A H 0.3630 -0.0126 1.1957 0.059 Uiso 1 1 calc R . . 
H18B H 0.3666 -0.0261 1.3308 0.059 Uiso 1 1 calc R . . 
H18C H 0.4360 -0.0993 1.2568 0.059 Uiso 1 1 calc R . . 
C19 C 0.5530(4) 0.1856(3) 1.3648(3) 0.0354(9) Uani 1 1 d . . . 
H19A H 0.5234 0.2314 1.3061 0.053 Uiso 0.50 1 calc PR . . 
H19B H 0.6319 0.2065 1.4019 0.053 Uiso 0.50 1 calc PR . . 
H19C H 0.4946 0.1809 1.4218 0.053 Uiso 0.50 1 calc PR . . 
H19A H 0.5765 0.1811 1.4471 0.053 Uiso 0.50 1 calc PR . . 
H19B H 0.4680 0.2060 1.3513 0.053 Uiso 0.50 1 calc PR . . 
H19C H 0.6053 0.2316 1.3314 0.053 Uiso 0.50 1 calc PR . . 
 
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 
Sn1 0.02496(18) 0.02519(18) 0.02710(17) -0.00107(10) 0.00525(11) -0.00090(9) 
Fe1 0.0225(3) 0.0253(3) 0.0273(3) -0.0049(2) 0.0031(2) -0.0005(2) 
Cl1 0.0480(6) 0.0412(6) 0.0324(5) 0.0060(4) 0.0035(5) 0.0117(5) 
C1 0.0238(19) 0.025(2) 0.0279(19) -0.0026(15) 0.0016(15) -0.0021(14) 
B1 0.027(2) 0.034(2) 0.025(2) -0.0018(18) -0.0003(17) -0.0078(18) 
C2 0.0229(18) 0.034(2) 0.0258(19) -0.0070(16) 0.0029(15) -0.0036(15) 
C3 0.0252(19) 0.036(2) 0.0267(19) -0.0115(16) 0.0061(16) -0.0039(16) 
C4 0.024(2) 0.033(2) 0.042(2) -0.0145(17) 0.0043(18) 0.0009(15) 
C5 0.0245(19) 0.023(2) 0.040(2) -0.0057(16) 0.0008(17) -0.0007(14) 
C6 0.032(2) 0.041(3) 0.039(2) -0.0162(19) 0.0063(18) -0.0021(18) 
C7 0.037(2) 0.029(2) 0.044(2) -0.0056(18) -0.0044(19) -0.0018(17) 
C8 0.032(2) 0.038(2) 0.041(2) -0.0055(18) 0.0053(17) -0.0138(18) 
C9 0.026(2) 0.040(2) 0.038(2) -0.0091(18) -0.0030(17) 0.0003(17) 
C10 0.029(2) 0.041(2) 0.034(2) -0.0048(18) -0.0051(17) -0.0033(17) 
C11 0.0245(18) 0.030(2) 0.0225(18) 0.0031(15) -0.0020(15) -0.0017(15) 
C12 0.0245(18) 0.029(2) 0.0284(19) -0.0038(16) 0.0018(15) -0.0002(15) 
C13 0.0284(19) 0.036(2) 0.038(2) -0.0022(18) 0.0047(17) -0.0030(17) 
C14 0.031(2) 0.042(3) 0.035(2) 0.0001(18) 0.0042(17) 0.0065(17) 
C15 0.043(2) 0.029(2) 0.036(2) -0.0010(17) 0.0016(18) 0.0018(18) 
C16 0.036(2) 0.029(2) 0.031(2) 0.0015(16) 0.0016(17) -0.0088(17) 
C17 0.0150(15) 0.0274(19) 0.0136(15) -0.0006(13) 0.0029(13) -0.0018(13) 
C18 0.033(2) 0.043(3) 0.044(2) 0.000(2) 0.0088(19) -0.0129(18) 
C19 0.038(2) 0.034(2) 0.035(2) -0.0078(17) 0.0053(17) 0.0064(18) 
 
_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 
Sn1 C19 2.121(4) . ? 
Sn1 C1 2.121(4) . ? 
Sn1 C18 2.130(4) . ? 
Sn1 Cl1 2.4036(12) . ? 
Fe1 C9 2.035(4) . ? 
Fe1 C3 2.035(4) . ? 
Fe1 C2 2.040(4) . ? 
Fe1 C8 2.045(4) . ? 
Fe1 C10 2.046(4) . ? 
Fe1 C1 2.052(4) . ? 
Fe1 C5 2.060(4) . ? 
Fe1 C7 2.061(4) . ? 
Fe1 C4 2.062(4) . ? 
Fe1 C6 2.063(4) . ? 
Fe1 B1 3.015(4) . ? 
C1 C5 1.427(5) . ? 
C1 C2 1.464(5) . ? 
B1 C2 1.536(6) . ? 
B1 C11 1.571(5) . ? 
B1 C17 1.623(5) . ? 
C2 C3 1.450(5) . ? 
C3 C4 1.414(6) . ? 
C4 C5 1.421(6) . ? 
C6 C7 1.407(6) . ? 
C6 C10 1.423(6) . ? 
C7 C8 1.418(6) . ? 
C8 C9 1.418(6) . ? 
C9 C10 1.405(6) . ? 
C11 C12 1.397(5) . ? 
C11 C16 1.407(5) . ? 
C12 C13 1.394(5) . ? 
C13 C14 1.376(6) . ? 
C14 C15 1.396(6) . ? 
C15 C16 1.380(6) . ? 
 
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 
C19 Sn1 C1 122.74(16) . . ? 
C19 Sn1 C18 116.08(17) . . ? 
C1 Sn1 C18 113.06(16) . . ? 
C19 Sn1 Cl1 99.54(12) . . ? 
C1 Sn1 Cl1 98.52(10) . . ? 
C18 Sn1 Cl1 100.65(13) . . ? 
C9 Fe1 C3 121.10(16) . . ? 
C9 Fe1 C2 158.74(16) . . ? 
C3 Fe1 C2 41.67(15) . . ? 
C9 Fe1 C8 40.69(17) . . ? 
C3 Fe1 C8 107.44(16) . . ? 
C2 Fe1 C8 123.54(16) . . ? 
C9 Fe1 C10 40.27(16) . . ? 
C3 Fe1 C10 156.24(16) . . ? 
C2 Fe1 C10 160.17(16) . . ? 
C8 Fe1 C10 68.10(17) . . ? 
C9 Fe1 C1 156.98(17) . . ? 
C3 Fe1 C1 69.51(15) . . ? 
C2 Fe1 C1 41.91(15) . . ? 
C8 Fe1 C1 161.22(16) . . ? 
C10 Fe1 C1 122.28(16) . . ? 
C9 Fe1 C5 120.64(16) . . ? 
C3 Fe1 C5 68.14(16) . . ? 
C2 Fe1 C5 69.23(16) . . ? 
C8 Fe1 C5 156.92(16) . . ? 
C10 Fe1 C5 106.33(17) . . ? 
C1 Fe1 C5 40.63(14) . . ? 
C9 Fe1 C7 67.82(17) . . ? 
C3 Fe1 C7 125.05(17) . . ? 
C2 Fe1 C7 109.65(16) . . ? 
C8 Fe1 C7 40.40(16) . . ? 
C10 Fe1 C7 67.64(17) . . ? 
C1 Fe1 C7 125.27(16) . . ? 
C5 Fe1 C7 160.18(16) . . ? 
C9 Fe1 C4 105.20(16) . . ? 
C3 Fe1 C4 40.36(17) . . ? 
C2 Fe1 C4 69.32(16) . . ? 
C8 Fe1 C4 121.65(16) . . ? 
C10 Fe1 C4 120.56(17) . . ? 
C1 Fe1 C4 68.76(15) . . ? 
C5 Fe1 C4 40.34(16) . . ? 
C7 Fe1 C4 159.18(17) . . ? 
C9 Fe1 C6 67.85(16) . . ? 
C3 Fe1 C6 161.46(17) . . ? 
C2 Fe1 C6 124.74(16) . . ? 
C8 Fe1 C6 67.83(17) . . ? 
C10 Fe1 C6 40.53(16) . . ? 
C1 Fe1 C6 108.85(16) . . ? 
C5 Fe1 C6 123.40(17) . . ? 
C7 Fe1 C6 39.88(17) . . ? 
C4 Fe1 C6 157.63(18) . . ? 
C9 Fe1 B1 141.86(15) . . ? 
C3 Fe1 B1 59.10(14) . . ? 
C2 Fe1 B1 27.69(14) . . ? 
C8 Fe1 B1 101.19(15) . . ? 
C10 Fe1 B1 143.91(15) . . ? 
C1 Fe1 B1 60.90(13) . . ? 
C5 Fe1 B1 95.60(14) . . ? 
C7 Fe1 B1 81.99(14) . . ? 
C4 Fe1 B1 94.73(14) . . ? 
C6 Fe1 B1 103.40(14) . . ? 
C5 C1 C2 107.3(3) . . ? 
C5 C1 Fe1 70.0(2) . . ? 
C2 C1 Fe1 68.6(2) . . ? 
C5 C1 Sn1 120.6(3) . . ? 
C2 C1 Sn1 131.9(3) . . ? 
Fe1 C1 Sn1 123.19(17) . . ? 
C2 B1 C11 120.4(3) . . ? 
C2 B1 C17 121.2(3) . . ? 
C11 B1 C17 118.3(3) . . ? 
C2 B1 Fe1 38.12(17) . . ? 
C11 B1 Fe1 122.9(2) . . ? 
C17 B1 Fe1 106.4(2) . . ? 
C3 C2 C1 106.2(3) . . ? 
C3 C2 B1 123.7(3) . . ? 
C1 C2 B1 128.2(3) . . ? 
C3 C2 Fe1 69.0(2) . . ? 
C1 C2 Fe1 69.5(2) . . ? 
B1 C2 Fe1 114.2(3) . . ? 
C4 C3 C2 109.1(3) . . ? 
C4 C3 Fe1 70.9(2) . . ? 
C2 C3 Fe1 69.4(2) . . ? 
C3 C4 C5 108.0(3) . . ? 
C3 C4 Fe1 68.8(2) . . ? 
C5 C4 Fe1 69.7(2) . . ? 
C4 C5 C1 109.3(4) . . ? 
C4 C5 Fe1 69.9(2) . . ? 
C1 C5 Fe1 69.4(2) . . ? 
C7 C6 C10 107.8(4) . . ? 
C7 C6 Fe1 70.0(2) . . ? 
C10 C6 Fe1 69.1(2) . . ? 
C6 C7 C8 108.5(4) . . ? 
C6 C7 Fe1 70.1(2) . . ? 
C8 C7 Fe1 69.2(2) . . ? 
C7 C8 C9 107.4(4) . . ? 
C7 C8 Fe1 70.4(2) . . ? 
C9 C8 Fe1 69.3(2) . . ? 
C10 C9 C8 108.4(4) . . ? 
C10 C9 Fe1 70.3(2) . . ? 
C8 C9 Fe1 70.0(2) . . ? 
C9 C10 C6 108.0(4) . . ? 
C9 C10 Fe1 69.4(2) . . ? 
C6 C10 Fe1 70.4(2) . . ? 
C12 C11 C16 117.1(3) . . ? 
C12 C11 B1 120.2(3) . . ? 
C16 C11 B1 122.5(3) . . ? 
C13 C12 C11 121.4(4) . . ? 
C14 C13 C12 120.3(4) . . ? 
C13 C14 C15 119.4(4) . . ? 
C16 C15 C14 120.2(4) . . ? 
C15 C16 C11 121.4(4) . . ? 
 
_diffrn_measured_fraction_theta_max    0.969 
_diffrn_reflns_theta_full              25.05 
_diffrn_measured_fraction_theta_full   0.969 
_refine_diff_density_max    0.707 
_refine_diff_density_min   -0.874 
_refine_diff_density_rms    0.097