# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2004 


data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'ProfD Guo-Xin Jin'
_publ_contact_author_address     
;
Department of Chemistry
Fudan University
Handan Road 220
Shanghai
200433
CHINA
;

_publ_contact_author_email       GXJIN@FUDAN.EDU.CN

_publ_section_title              
;
Phenyl thiolate as a sigma- and pi- donor ligand:
synthesis of a 3-D organometallic coordination polymer [K2Fe(SPh)4]n
;
loop_
_publ_author_name
'Guo-Xin Jin'
'Lin-Hong Weng'
'Xiao-Yan Yu'

data_complex_1
_database_code_depnum_ccdc_archive 'CCDC 234591'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H20 Fe K2 S4'
_chemical_formula_sum            'C24 H20 Fe K2 S4'
_chemical_formula_weight         570.69

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'
K K 0.2009 0.2494 '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'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   'I-42d '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y, -z+3/4'
'x+1/2, -y, -z+3/4'
'-y+1/2, -x, z+3/4'
'y+1/2, x, z+3/4'
'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'
'-x+1, y+1/2, -z+5/4'
'x+1, -y+1/2, -z+5/4'
'-y+1, -x+1/2, z+5/4'
'y+1, x+1/2, z+5/4'

_cell_length_a                   12.580(6)
_cell_length_b                   12.580(6)
_cell_length_c                   16.127(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2552(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    320
_cell_measurement_theta_min      2.384
_cell_measurement_theta_max      26.644

_exptl_crystal_description       block
_exptl_crystal_colour            brown-yellow
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1168
_exptl_absorpt_coefficient_mu    1.255
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6021
_exptl_absorpt_correction_T_max  0.7444
_exptl_absorpt_process_details   psi-scan

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_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  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5983
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.05
_diffrn_reflns_theta_max         27.11
_reflns_number_total             1411
_reflns_number_gt                1319
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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^)+(0.0614P)^2^+0.2046P] 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    constall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.17(4)
_refine_ls_number_reflns         1411
_refine_ls_number_parameters     71
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0445
_refine_ls_wR_factor_ref         0.1264
_refine_ls_wR_factor_gt          0.1235
_refine_ls_goodness_of_fit_ref   1.449
_refine_ls_restrained_S_all      1.449
_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
Fe1 Fe 1.0000 0.5000 0.2500 0.0330(3) Uani 1 4 d S . .
S1 S 0.87491(10) 0.60236(9) 0.17856(8) 0.0574(3) Uani 1 1 d . . .
C1 C 0.8106(3) 0.5072(4) 0.1142(3) 0.0483(9) Uani 1 1 d . . .
K1 K 0.91091(13) 0.2500 0.1250 0.0608(4) Uani 1 2 d S . .
C2 C 0.7189(4) 0.4554(5) 0.1411(3) 0.0656(13) Uani 1 1 d . . .
H2A H 0.6923 0.4688 0.1939 0.079 Uiso 1 1 calc R . .
C3 C 0.6666(5) 0.3834(6) 0.0890(4) 0.0861(19) Uani 1 1 d . . .
H3A H 0.6051 0.3498 0.1072 0.103 Uiso 1 1 calc R . .
C4 C 0.7059(5) 0.3618(6) 0.0105(4) 0.0851(19) Uani 1 1 d . . .
H4A H 0.6647 0.3178 -0.0280 0.102 Uiso 1 1 calc R . .
C5 C 0.7965(5) 0.4112(6) -0.0159(4) 0.0786(16) Uani 1 1 d . . .
H5A H 0.8173 0.4054 -0.0742 0.094 Uiso 1 1 calc R . .
C6 C 0.8476(4) 0.4842(4) 0.0345(3) 0.0613(12) Uani 1 1 d . . .
H6A H 0.9045 0.5279 0.0109 0.074 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
Fe1 0.0294(3) 0.0294(3) 0.0404(5) 0.000 0.000 0.000
S1 0.0540(6) 0.0430(6) 0.0754(8) 0.0058(5) -0.0149(5) -0.0013(5)
C1 0.0447(19) 0.0405(19) 0.060(2) 0.006(2) -0.0078(17) -0.0002(18)
K1 0.0646(9) 0.0536(8) 0.0642(8) 0.0028(7) 0.000 0.000
C2 0.064(3) 0.071(3) 0.062(3) -0.003(2) 0.005(2) -0.012(2)
C3 0.065(3) 0.093(5) 0.100(4) 0.004(4) -0.003(3) -0.029(3)
C4 0.085(4) 0.085(4) 0.085(4) -0.007(3) -0.027(3) -0.018(3)
C5 0.085(4) 0.094(4) 0.056(3) 0.003(3) -0.014(3) 0.002(3)
C6 0.060(3) 0.063(3) 0.061(2) 0.010(2) -0.007(2) 0.001(2)

_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
Fe1 S1 2.3371(14) 11_565 ?
Fe1 S1 2.3371(14) 2_765 ?
Fe1 S1 2.3371(14) . ?
Fe1 S1 2.3371(14) 12_645 ?
Fe1 K1 3.9001(15) . ?
Fe1 K1 3.9001(15) 2_765 ?
Fe1 K1 3.9001(15) 12_645 ?
Fe1 K1 3.9001(15) 11_565 ?
S1 C1 1.779(4) . ?
S1 K1 3.385(2) 2_765 ?
S1 K1 3.540(2) 11_565 ?
C1 C2 1.394(6) . ?
C1 C6 1.398(7) . ?
C1 K1 3.477(5) . ?
K1 C5 3.368(6) . ?
K1 C5 3.368(6) 14_454 ?
K1 C6 3.383(5) . ?
K1 C6 3.383(5) 14_454 ?
K1 S1 3.385(2) 2_765 ?
K1 S1 3.385(2) 13_644 ?
K1 C4 3.470(7) . ?
K1 C4 3.470(7) 14_454 ?
K1 C1 3.477(5) 14_454 ?
K1 S1 3.540(2) 7_664 ?
K1 S1 3.540(2) 12_645 ?
C2 C3 1.399(8) . ?
C3 C4 1.385(10) . ?
C4 C5 1.365(9) . ?
C5 C6 1.384(8) . ?

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
S1 Fe1 S1 104.07(3) 11_565 2_765 ?
S1 Fe1 S1 104.07(3) 11_565 . ?
S1 Fe1 S1 120.93(8) 2_765 . ?
S1 Fe1 S1 120.93(8) 11_565 12_645 ?
S1 Fe1 S1 104.07(3) 2_765 12_645 ?
S1 Fe1 S1 104.07(3) . 12_645 ?
S1 Fe1 K1 162.96(3) 11_565 . ?
S1 Fe1 K1 59.63(4) 2_765 . ?
S1 Fe1 K1 89.77(4) . . ?
S1 Fe1 K1 63.48(5) 12_645 . ?
S1 Fe1 K1 63.48(5) 11_565 2_765 ?
S1 Fe1 K1 89.77(4) 2_765 2_765 ?
S1 Fe1 K1 59.63(4) . 2_765 ?
S1 Fe1 K1 162.96(3) 12_645 2_765 ?
K1 Fe1 K1 117.76(4) . 2_765 ?
S1 Fe1 K1 59.63(4) 11_565 12_645 ?
S1 Fe1 K1 63.48(5) 2_765 12_645 ?
S1 Fe1 K1 162.96(3) . 12_645 ?
S1 Fe1 K1 89.77(4) 12_645 12_645 ?
K1 Fe1 K1 105.495(18) . 12_645 ?
K1 Fe1 K1 105.495(18) 2_765 12_645 ?
S1 Fe1 K1 89.77(4) 11_565 11_565 ?
S1 Fe1 K1 162.96(3) 2_765 11_565 ?
S1 Fe1 K1 63.48(5) . 11_565 ?
S1 Fe1 K1 59.63(4) 12_645 11_565 ?
K1 Fe1 K1 105.495(18) . 11_565 ?
K1 Fe1 K1 105.495(18) 2_765 11_565 ?
K1 Fe1 K1 117.76(4) 12_645 11_565 ?
C1 S1 Fe1 102.88(14) . . ?
C1 S1 K1 125.63(15) . 2_765 ?
Fe1 S1 K1 83.81(4) . 2_765 ?
C1 S1 K1 106.76(15) . 11_565 ?
Fe1 S1 K1 80.31(5) . 11_565 ?
K1 S1 K1 127.41(4) 2_765 11_565 ?
C2 C1 C6 117.7(4) . . ?
C2 C1 S1 120.6(4) . . ?
C6 C1 S1 121.7(3) . . ?
C2 C1 K1 81.4(3) . . ?
C6 C1 K1 74.5(3) . . ?
S1 C1 K1 115.61(17) . . ?
C5 K1 C5 129.4(2) . 14_454 ?
C5 K1 C6 23.66(14) . . ?
C5 K1 C6 135.61(15) 14_454 . ?
C5 K1 C6 135.61(15) . 14_454 ?
C5 K1 C6 23.66(14) 14_454 14_454 ?
C6 K1 C6 152.75(19) . 14_454 ?
C5 K1 S1 100.49(11) . 2_765 ?
C5 K1 S1 119.91(11) 14_454 2_765 ?
C6 K1 S1 79.62(9) . 2_765 ?
C6 K1 S1 123.73(10) 14_454 2_765 ?
C5 K1 S1 119.91(11) . 13_644 ?
C5 K1 S1 100.49(11) 14_454 13_644 ?
C6 K1 S1 123.73(10) . 13_644 ?
C6 K1 S1 79.62(9) 14_454 13_644 ?
S1 K1 S1 74.49(5) 2_765 13_644 ?
C5 K1 C4 22.97(15) . . ?
C5 K1 C4 106.58(18) 14_454 . ?
C6 K1 C4 40.73(14) . . ?
C6 K1 C4 114.06(15) 14_454 . ?
S1 K1 C4 120.33(11) 2_765 . ?
S1 K1 C4 132.72(13) 13_644 . ?
C5 K1 C4 106.58(18) . 14_454 ?
C5 K1 C4 22.97(15) 14_454 14_454 ?
C6 K1 C4 114.06(15) . 14_454 ?
C6 K1 C4 40.73(14) 14_454 14_454 ?
S1 K1 C4 132.72(13) 2_765 14_454 ?
S1 K1 C4 120.33(11) 13_644 14_454 ?
C4 K1 C4 84.0(3) . 14_454 ?
C5 K1 C1 116.03(13) . 14_454 ?
C5 K1 C1 41.50(13) 14_454 14_454 ?
C6 K1 C1 138.28(12) . 14_454 ?
C6 K1 C1 23.46(11) 14_454 14_454 ?
S1 K1 C1 141.88(8) 2_765 14_454 ?
S1 K1 C1 77.93(7) 13_644 14_454 ?
C4 K1 C1 97.71(14) . 14_454 ?
C4 K1 C1 47.66(13) 14_454 14_454 ?
C5 K1 C1 41.50(13) . . ?
C5 K1 C1 116.03(13) 14_454 . ?
C6 K1 C1 23.46(11) . . ?
C6 K1 C1 138.28(12) 14_454 . ?
S1 K1 C1 77.93(7) 2_765 . ?
S1 K1 C1 141.88(8) 13_644 . ?
C4 K1 C1 47.66(13) . . ?
C4 K1 C1 97.71(14) 14_454 . ?
C1 K1 C1 137.45(14) 14_454 . ?
C5 K1 S1 69.12(12) . 7_664 ?
C5 K1 S1 108.43(12) 14_454 7_664 ?
C6 K1 S1 89.39(9) . 7_664 ?
C6 K1 S1 89.34(10) 14_454 7_664 ?
S1 K1 S1 120.63(5) 2_765 7_664 ?
S1 K1 S1 64.25(3) 13_644 7_664 ?
C4 K1 S1 70.65(13) . 7_664 ?
C4 K1 S1 105.14(13) 14_454 7_664 ?
C1 K1 S1 67.33(7) 14_454 7_664 ?
C1 K1 S1 110.56(7) . 7_664 ?
C5 K1 S1 108.43(12) . 12_645 ?
C5 K1 S1 69.12(12) 14_454 12_645 ?
C6 K1 S1 89.34(10) . 12_645 ?
C6 K1 S1 89.39(9) 14_454 12_645 ?
S1 K1 S1 64.25(3) 2_765 12_645 ?
S1 K1 S1 120.63(5) 13_644 12_645 ?
C4 K1 S1 105.14(13) . 12_645 ?
C4 K1 S1 70.65(13) 14_454 12_645 ?
C1 K1 S1 110.56(7) 14_454 12_645 ?
C1 K1 S1 67.33(7) . 12_645 ?
S1 K1 S1 174.60(6) 7_664 12_645 ?
C1 C2 C3 120.3(5) . . ?
C4 C3 C2 120.5(6) . . ?
C5 C4 C3 119.5(6) . . ?
C5 C4 K1 74.3(4) . . ?
C3 C4 K1 81.8(4) . . ?
C4 C5 C6 120.4(6) . . ?
C4 C5 K1 82.7(4) . . ?
C6 C5 K1 78.8(3) . . ?
C5 C6 C1 121.5(5) . . ?
C5 C6 K1 77.6(3) . . ?
C1 C6 K1 82.0(3) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.11
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.079
#-----------------END