#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:50:29 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180157 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/53/7105396.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_7105396
loop_
_publ_author_name
'Pöhlker, Christopher'
'Schellenberg, Inga'
'Pöttgen, Rainer'
'Dehnen, Stefanie'
_publ_section_title
;
 Synthesis and reactivity of ferrocenyl functionalized Sn/S cages
;
_journal_issue                   15
_journal_name_full               'Chemical Communications'
_journal_page_first              2605
_journal_paper_doi               10.1039/b923871a
_journal_volume                  46
_journal_year                    2010
_chemical_formula_moiety         'C40 H36 Fe4 S6 Sn4'
_chemical_formula_sum            'C40 H36 Fe4 S6 Sn4'
_chemical_formula_weight         1407.21
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.967(3)
_cell_length_b                   13.967(3)
_cell_length_c                   11.064(2)
_cell_measurement_reflns_used    25222
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      54.12
_cell_measurement_theta_min      9.83
_cell_volume                     2158.3(8)
_computing_cell_refinement       'XAREA 1.38 (Stoe 2006)'
_computing_data_collection       'XAREA 1.38 (Stoe 2006)'
_computing_data_reduction        'XAREA 1.38 (Stoe 2006)'
_computing_molecular_graphics
'DIAMOND 3.0 (Brandenburg & Putz, 2005) SHELXTL-NT V5.1, Bruker AXS 1999'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  IPDS2
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_av_sigmaI/netI    0.0146
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8638
_diffrn_reflns_theta_full        26.77
_diffrn_reflns_theta_max         26.77
_diffrn_reflns_theta_min         4.92
_exptl_absorpt_coefficient_mu    3.899
_exptl_absorpt_correction_T_max  0.281
_exptl_absorpt_correction_T_min  0.235
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'XPREP in SHELXTL (Bruker, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.165
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.25
_refine_diff_density_min         -0.66
_refine_diff_density_rms         0.07
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         2256
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0162
_refine_ls_R_factor_gt           0.0157
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0300P)²+1.3140P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0429
_refine_ls_wR_factor_ref         0.0431
_reflns_number_gt                2228
_reflns_number_total             2256
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b923871a.txt
_cod_data_source_block           3abs
_cod_database_code               7105396
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+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
Sn1 Sn 0.376377(11) 0.555988(11) 0.378609(18) 0.01595(6) Uani 1 1 d . . .
Fe1 Fe 0.21124(3) 0.53134(3) 0.13116(4) 0.02261(10) Uani 1 1 d . . .
S1 S 0.31154(5) 0.43119(5) 0.50158(6) 0.02112(15) Uani 1 1 d . . .
S2 S 0.5000 0.5000 0.24543(8) 0.02164(19) Uani 1 2 d S . .
C1 C 0.2586(2) 0.6047(2) 0.2788(2) 0.0196(6) Uani 1 1 d . . .
C2 C 0.1617(2) 0.5727(3) 0.2958(3) 0.0278(7) Uani 1 1 d . . .
H2 H 0.1399 0.5313 0.3581 0.033 Uiso 1 1 calc R . .
C3 C 0.1047(2) 0.6133(3) 0.2037(3) 0.0360(8) Uani 1 1 d . . .
H3 H 0.0378 0.6039 0.1935 0.043 Uiso 1 1 calc R . .
C4 C 0.1647(2) 0.6709(2) 0.1283(4) 0.0333(6) Uani 1 1 d . . .
H4 H 0.1447 0.7066 0.0597 0.040 Uiso 1 1 calc R . .
C5 C 0.2598(2) 0.6652(2) 0.1744(3) 0.0256(7) Uani 1 1 d . . .
H5 H 0.3145 0.6962 0.1415 0.031 Uiso 1 1 calc R . .
C6 C 0.2839(2) 0.4034(2) 0.1168(4) 0.0330(7) Uani 1 1 d . . .
H6 H 0.3256 0.3761 0.1753 0.040 Uiso 1 1 calc R . .
C7 C 0.1840(3) 0.3886(2) 0.1092(4) 0.0425(9) Uani 1 1 d . . .
H7 H 0.1466 0.3504 0.1623 0.051 Uiso 1 1 calc R . .
C8 C 0.1495(3) 0.4402(3) 0.0093(4) 0.0493(11) Uani 1 1 d . . .
H8 H 0.0850 0.4419 -0.0179 0.059 Uiso 1 1 calc R . .
C9 C 0.2274(3) 0.4892(3) -0.0435(3) 0.0447(10) Uani 1 1 d . . .
H9 H 0.2244 0.5306 -0.1115 0.054 Uiso 1 1 calc R . .
C10 C 0.3108(3) 0.4655(3) 0.0229(3) 0.0341(8) Uani 1 1 d . . .
H10 H 0.3738 0.4878 0.0068 0.041 Uiso 1 1 calc R . .
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'
S S 0.1246 0.1234 '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'
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 Sn1 S1 103.85(9) . . ?
C1 Sn1 S2 110.32(8) . . ?
S1 Sn1 S2 112.61(2) . . ?
C1 Sn1 S1 106.92(8) . 3_566 ?
S1 Sn1 S1 111.63(2) . 3_566 ?
S2 Sn1 S1 111.13(2) . 3_566 ?
C2 Fe1 C9 166.45(16) . . ?
C2 Fe1 C1 41.34(12) . . ?
C9 Fe1 C1 150.63(17) . . ?
C2 Fe1 C3 40.57(14) . . ?
C9 Fe1 C3 128.07(15) . . ?
C1 Fe1 C3 68.89(12) . . ?
C2 Fe1 C7 108.68(17) . . ?
C9 Fe1 C7 67.98(19) . . ?
C1 Fe1 C7 130.23(16) . . ?
C3 Fe1 C7 117.23(16) . . ?
C2 Fe1 C8 128.63(18) . . ?
C9 Fe1 C8 40.50(19) . . ?
C1 Fe1 C8 167.96(17) . . ?
C3 Fe1 C8 107.47(16) . . ?
C7 Fe1 C8 40.19(18) . . ?
C2 Fe1 C5 69.12(14) . . ?
C9 Fe1 C5 116.76(17) . . ?
C1 Fe1 C5 41.04(12) . . ?
C3 Fe1 C5 68.75(15) . . ?
C7 Fe1 C5 168.81(15) . . ?
C8 Fe1 C5 149.63(16) . . ?
C2 Fe1 C10 151.75(14) . . ?
C9 Fe1 C10 40.57(15) . . ?
C1 Fe1 C10 118.23(14) . . ?
C3 Fe1 C10 166.95(15) . . ?
C7 Fe1 C10 67.67(16) . . ?
C8 Fe1 C10 67.81(17) . . ?
C5 Fe1 C10 108.73(15) . . ?
C2 Fe1 C4 68.70(15) . . ?
C9 Fe1 C4 107.16(17) . . ?
C1 Fe1 C4 68.80(14) . . ?
C3 Fe1 C4 40.87(16) . . ?
C7 Fe1 C4 149.79(14) . . ?
C8 Fe1 C4 116.51(15) . . ?
C5 Fe1 C4 40.68(13) . . ?
C10 Fe1 C4 129.05(16) . . ?
C2 Fe1 C6 118.87(15) . . ?
C9 Fe1 C6 67.74(16) . . ?
C1 Fe1 C6 109.75(13) . . ?
C3 Fe1 C6 151.04(16) . . ?
C7 Fe1 C6 40.25(13) . . ?
C8 Fe1 C6 67.50(15) . . ?
C5 Fe1 C6 130.35(13) . . ?
C10 Fe1 C6 39.95(16) . . ?
C4 Fe1 C6 167.69(15) . . ?
Sn1 S1 Sn1 104.77(3) . 4_656 ?
Sn1 S2 Sn1 104.28(4) . 2_665 ?
C5 C1 C2 107.5(3) . . ?
C5 C1 Fe1 69.75(17) . . ?
C2 C1 Fe1 69.06(17) . . ?
C5 C1 Sn1 127.4(2) . . ?
C2 C1 Sn1 124.7(2) . . ?
Fe1 C1 Sn1 120.91(14) . . ?
C3 C2 C1 108.2(3) . . ?
C3 C2 Fe1 70.09(18) . . ?
C1 C2 Fe1 69.60(17) . . ?
C3 C2 H2 125.9 . . ?
C1 C2 H2 125.9 . . ?
Fe1 C2 H2 126.0 . . ?
C2 C3 C4 108.4(3) . . ?
C2 C3 Fe1 69.33(19) . . ?
C4 C3 Fe1 70.1(2) . . ?
C2 C3 H3 125.8 . . ?
C4 C3 H3 125.8 . . ?
Fe1 C3 H3 126.4 . . ?
C5 C4 C3 107.8(3) . . ?
C5 C4 Fe1 69.31(18) . . ?
C3 C4 Fe1 69.05(19) . . ?
C5 C4 H4 126.1 . . ?
C3 C4 H4 126.1 . . ?
Fe1 C4 H4 127.1 . . ?
C4 C5 C1 108.1(3) . . ?
C4 C5 Fe1 70.01(17) . . ?
C1 C5 Fe1 69.21(17) . . ?
C4 C5 H5 126.0 . . ?
C1 C5 H5 126.0 . . ?
Fe1 C5 H5 126.4 . . ?
C10 C6 C7 108.1(4) . . ?
C10 C6 Fe1 69.68(18) . . ?
C7 C6 Fe1 69.23(18) . . ?
C10 C6 H6 126.0 . . ?
C7 C6 H6 126.0 . . ?
Fe1 C6 H6 126.7 . . ?
C8 C7 C6 108.1(4) . . ?
C8 C7 Fe1 69.9(2) . . ?
C6 C7 Fe1 70.52(18) . . ?
C8 C7 H7 126.0 . . ?
C6 C7 H7 126.0 . . ?
Fe1 C7 H7 125.2 . . ?
C7 C8 C9 108.1(3) . . ?
C7 C8 Fe1 69.9(2) . . ?
C9 C8 Fe1 69.3(2) . . ?
C7 C8 H8 126.0 . . ?
C9 C8 H8 126.0 . . ?
Fe1 C8 H8 126.4 . . ?
C8 C9 C10 107.8(3) . . ?
C8 C9 Fe1 70.2(2) . . ?
C10 C9 Fe1 70.45(19) . . ?
C8 C9 H9 126.1 . . ?
C10 C9 H9 126.1 . . ?
Fe1 C9 H9 124.9 . . ?
C6 C10 C9 107.9(4) . . ?
C6 C10 Fe1 70.37(19) . . ?
C9 C10 Fe1 69.0(2) . . ?
C6 C10 H10 126.0 . . ?
C9 C10 H10 126.0 . . ?
Fe1 C10 H10 126.2 . . ?
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
Sn1 C1 2.095(3) . ?
Sn1 S1 2.3894(8) . ?
Sn1 S2 2.4009(7) . ?
Sn1 S1 2.4014(8) 3_566 ?
Fe1 C2 2.032(3) . ?
Fe1 C9 2.033(3) . ?
Fe1 C1 2.039(3) . ?
Fe1 C3 2.042(3) . ?
Fe1 C7 2.044(3) . ?
Fe1 C8 2.045(3) . ?
Fe1 C5 2.046(3) . ?
Fe1 C10 2.052(3) . ?
Fe1 C4 2.055(3) . ?
Fe1 C6 2.061(3) . ?
S1 Sn1 2.4014(8) 4_656 ?
S2 Sn1 2.4009(7) 2_665 ?
C1 C5 1.432(4) . ?
C1 C2 1.437(4) . ?
C2 C3 1.412(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.431(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.426(5) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C10 1.405(5) . ?
C6 C7 1.413(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.405(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.411(7) . ?
C8 H8 0.9500 . ?
C9 C10 1.417(5) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
