#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:16:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179320 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/17/4321754.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_4321754
loop_
_publ_author_name
'Dieter Sellmann'
'Jürgen Utz'
'Frank W. Heinemann'
_publ_contact_author
; 
        Prof. Dr. D. Sellmann 
        Institut für Anorganische Chemie II 
        Universität Erlangen-Nürnberg 
        Egerlandstr. 1 
        D-91058 Erlangen 
        Bundesrepublik Deutschland 
;
_publ_contact_author_email       SELLMANN@ANORGANIK.CHEMIE.UNI-ERLANGEN.DE
_publ_contact_author_fax         '049 9131 85-7367'
_publ_contact_author_phone       '049 9131 85-7360'
_publ_section_title
;
 Transition-Metal Complexes with Sulfur Ligands. 132.1 Electron-Rich Fe
 and Ru Complexes with [MN₂S₃] Cores Containing the New Pentadentate
 Ligand 'N₂H₂S₃'²⁻ (= 2,2'-Bis(2-mercaptophenylamino)diethyl
 Sulfide(2-))
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              459
_journal_page_last               466
_journal_paper_doi               10.1021/ic980383q
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C17 H18 Fe N2 O S3'
_chemical_formula_weight         418.36
_chemical_name_systematic
;                                                                               
 ?                                                                              
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 95.36(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.136(8)
_cell_length_b                   11.406(15)
_cell_length_c                   19.871(18)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      18.0
_cell_measurement_theta_min      13.0
_cell_volume                     1836(3)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'Siemens XDISK'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  'CIFTAB (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL PLUS 4.21/V'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'omega scans'
_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  0.1027
_diffrn_reflns_av_sigmaI/netI    0.0643
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            5010
_diffrn_reflns_theta_max         27.09
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        99.8
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.169
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_description       columns
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.516
_refine_diff_density_min         -1.110
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.059
_refine_ls_goodness_of_fit_obs   1.086
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         4028
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_restrained_S_obs      1.086
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_obs          0.0415
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0639P)²+1.0635P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1424
_refine_ls_wR_factor_obs         0.1099
_reflns_number_observed          2741
_reflns_number_total             4030
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980383q_3.cif
_cod_data_source_block           ju32
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0639P)^2^+1.0635P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0639P)^2^+1.0635P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1835.9(34)
_cod_database_code               4321754
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'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Fe1 Fe 0.18491(6) 0.10746(5) 0.29985(3) 0.0226(2) Uani 1 d . .
C1 C 0.2090(5) 0.1919(3) 0.3740(2) 0.0277(8) Uani 1 d . .
O1 O 0.2212(4) 0.2494(3) 0.42321(15) 0.0460(8) Uani 1 d . .
S1 S -0.01306(11) 0.00344(9) 0.34979(5) 0.0287(2) Uani 1 d . .
S2 S 0.39732(12) 0.19124(9) 0.25018(5) 0.0310(2) Uani 1 d . .
S3 S -0.00325(12) 0.24174(9) 0.25081(5) 0.0273(2) Uani 1 d . .
N1 N 0.3514(4) -0.0198(3) 0.33717(15) 0.0228(6) Uani 1 d . .
N2 N 0.1349(4) 0.0094(3) 0.21071(15) 0.0254(7) Uani 1 d . .
C15 C 0.2963(5) -0.0800(3) 0.3981(2) 0.0266(8) Uani 1 d . .
C14 C 0.4065(5) -0.1449(4) 0.4420(2) 0.0315(9) Uani 1 d . .
C13 C 0.3486(5) -0.2065(4) 0.4965(2) 0.0373(10) Uani 1 d . .
C12 C 0.1818(6) -0.1994(4) 0.5084(2) 0.0387(10) Uani 1 d . .
C11 C 0.0714(5) -0.1343(4) 0.4644(2) 0.0321(9) Uani 1 d . .
C10 C 0.1264(5) -0.0747(4) 0.4077(2) 0.0279(8) Uani 1 d . .
C25 C -0.0143(5) 0.0479(4) 0.1672(2) 0.0288(8) Uani 1 d . .
C24 C -0.0765(6) -0.0216(4) 0.1125(2) 0.0439(11) Uani 1 d . .
C23 C -0.2097(6) 0.0183(4) 0.0679(2) 0.0421(11) Uani 1 d . .
C22 C -0.2790(5) 0.1275(4) 0.0791(2) 0.0361(10) Uani 1 d . .
C21 C -0.2193(5) 0.1979(4) 0.1347(2) 0.0293(8) Uani 1 d . .
C20 C -0.0840(4) 0.1585(4) 0.1800(2) 0.0277(8) Uani 1 d . .
C16 C 0.5235(5) 0.0335(3) 0.3495(2) 0.0297(8) Uani 1 d . .
C17 C 0.5689(5) 0.0944(4) 0.2853(2) 0.0369(10) Uani 1 d . .
C26 C 0.2824(5) 0.0065(4) 0.1693(2) 0.0327(9) Uani 1 d . .
C27 C 0.3521(5) 0.1277(4) 0.1646(2) 0.0363(10) Uani 1 d . .
H1 H 0.3542 -0.0857 0.3022 0.050 Uiso 1 d . .
H2 H 0.1118 -0.0795 0.2214 0.050 Uiso 1 d . .
H14 H 0.5218 -0.1463 0.4365 0.050 Uiso 1 d . .
H13 H 0.4393 -0.2566 0.5243 0.050 Uiso 1 d . .
H12 H 0.1275 -0.2507 0.5449 0.050 Uiso 1 d . .
H11 H -0.0417 -0.1052 0.4762 0.050 Uiso 1 d . .
H24 H -0.0264 -0.1074 0.1025 0.050 Uiso 1 d . .
H23 H -0.3705 0.1668 0.0425 0.050 Uiso 1 d . .
H22 H -0.2511 -0.0368 0.0228 0.050 Uiso 1 d . .
H21 H -0.2792 0.2812 0.1429 0.050 Uiso 1 d . .
H16A H 0.5992 -0.0311 0.3598 0.050 Uiso 1 d . .
H16B H 0.5204 0.1029 0.3828 0.050 Uiso 1 d . .
H17A H 0.6710 0.1453 0.2953 0.050 Uiso 1 d . .
H17B H 0.5860 0.0437 0.2435 0.050 Uiso 1 d . .
H26A H 0.3647 -0.0479 0.1945 0.050 Uiso 1 d . .
H26B H 0.2453 -0.0240 0.1225 0.050 Uiso 1 d . .
H27A H 0.2833 0.1912 0.1458 0.050 Uiso 1 d . .
H27B H 0.4527 0.1161 0.1465 0.050 Uiso 1 d . .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
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 Fe1 N1 93.8(2) . . ?
C1 Fe1 N2 175.2(2) . . ?
N1 Fe1 N2 89.85(14) . . ?
C1 Fe1 S2 95.97(14) . . ?
N1 Fe1 S2 87.25(11) . . ?
N2 Fe1 S2 87.30(11) . . ?
C1 Fe1 S1 87.04(14) . . ?
N1 Fe1 S1 86.85(12) . . ?
N2 Fe1 S1 90.05(12) . . ?
S2 Fe1 S1 173.54(4) . . ?
C1 Fe1 S3 90.48(15) . . ?
N1 Fe1 S3 175.76(9) . . ?
N2 Fe1 S3 85.92(12) . . ?
S2 Fe1 S3 92.21(8) . . ?
S1 Fe1 S3 93.48(8) . . ?
O1 C1 Fe1 178.3(4) . . ?
C10 S1 Fe1 96.18(15) . . ?
C27 S2 C17 100.9(2) . . ?
C27 S2 Fe1 98.0(2) . . ?
C17 S2 Fe1 99.3(2) . . ?
C20 S3 Fe1 99.3(2) . . ?
C15 N1 C16 113.1(3) . . ?
C15 N1 Fe1 112.0(2) . .. ?
C16 N1 Fe1 109.7(2) . . ?
C25 N2 C26 109.6(3) . . ?
C25 N2 Fe1 114.6(2) . . ?
C26 N2 Fe1 111.6(2) . . ?
C14 C15 C10 121.0(4) . . ?
C14 C15 N1 121.5(3) . . ?
C10 C15 N1 117.4(3) . . ?
C15 C14 C13 120.1(4) . . ?
C12 C13 C14 119.9(4) . . ?
C13 C12 C11 119.9(4) . . ?
C12 C11 C10 121.0(4) . . ?
C15 C10 C11 118.0(4) . . ?
C15 C10 S1 120.4(3) . . ?
C11 C10 S1 121.5(3) . . ?
C24 C25 C20 121.5(4) . . ?
C24 C25 N2 119.9(4) . . ?
C20 C25 N2 118.5(3) . . ?
C25 C24 C23 120.4(4) . . ?
C22 C23 C24 119.1(4) . . ?
C23 C22 C21 121.2(4) . . ?
C22 C21 C20 120.1(4) . . ?
C25 C20 C21 117.7(3) . . ?
C25 C20 S3 119.7(3) . . ?
C21 C20 S3 122.6(3) . . ?
N1 C16 C17 109.7(3) .. . ?
C16 C17 S2 110.5(3) . . ?
C27 C26 N2 109.7(3) . . ?
C26 C27 S2 110.2(3) . . ?
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 C1 1.756(4) . ?
Fe1 N1 2.075(3) . ?
Fe1 N2 2.102(3) . ?
Fe1 S2 2.279(2) . ?
Fe1 S1 2.299(2) . ?
Fe1 S3 2.315(2) . ?
C1 O1 1.173(5) . ?
S1 C10 1.779(4) . ?
S2 C27 1.854(5) . ?
S2 C17 1.864(4) . ?
S3 C20 1.773(4) . ?
N1 C15 1.497(5) . ?
N1 C16 1.525(5) . ?
N2 C25 1.490(5) . ?
N2 C26 1.517(5) . ?
C15 C14 1.401(5) . ?
C15 C10 1.414(5) . ?
C14 C13 1.409(6) . ?
C13 C12 1.402(6) . ?
C12 C11 1.405(6) . ?
C11 C10 1.423(5) . ?
C25 C24 1.401(6) . ?
C25 C20 1.416(6) . ?
C24 C23 1.410(6) . ?
C23 C22 1.394(6) . ?
C22 C21 1.414(6) . ?
C21 C20 1.428(5) . ?
C16 C17 1.528(6) . ?
C26 C27 1.501(6) . ?
