#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:32:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179145 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/06/4310619.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_4310619
loop_
_publ_author_name
'Athanassios K. Boudalis'
'Juan-Modesto Clemente-Juan'
'Françoise Dahan'
'Jean-Pierre Tuchagues'
_publ_contact_author
;
       Pr Jean-Pierre Tuchagues
       Laboratoire de Chimie de Coordination du CNRS
       205 Route de Narbonne
       31077 Toulouse Cedex 4
       France
;
_publ_contact_author_email       tuchague@lcctoul.lcc-toulouse.fr
_publ_contact_author_fax         '(33) 0561553003'
_publ_contact_author_phone       '(33) 0561333154'
_publ_section_title
;
 New Poly-Iron(II) Complexes of N4O Dinucleating Schiff Bases and
 Pseudohalides: Syntheses, Structures, and Magnetic and Mössbauer
 Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1574
_journal_page_last               1586
_journal_paper_doi               10.1021/ic0351904
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C23 H26 Fe2 N6 O3 S2'
_chemical_formula_weight         610.32
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.180(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0380(7)
_cell_length_b                   12.4495(8)
_cell_length_c                   27.358(2)
_cell_measurement_temperature    180(2)
_cell_volume                     2735.7(4)
_computing_cell_refinement       'STOE-IPDS software (Stoe, 2.93, 1997)'
_computing_data_collection       'STOE-IPDS software (Stoe, 2.93, 1997)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_computing_molecular_graphics    'ZORTEP (Zsolnai, 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  STOE-IPDS
_diffrn_measurement_method       'Imaging Plate Detector System'
_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  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            21502
_diffrn_reflns_theta_full        26.03
_diffrn_reflns_theta_max         26.03
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    1.249
_exptl_absorpt_correction_T_max  0.8783
_exptl_absorpt_correction_T_min  0.5671
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-SHAPE (Stoe & Cie, 1996)'
_exptl_crystal_colour            Blue-Black
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5363
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0322P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0672
_reflns_number_gt                3843
_reflns_number_total             5363
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0351904si20040114_092725_1.cif
_cod_data_source_block           (1)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+0.0000P] 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^)+(0.0322P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4310619
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_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.63963(3) 0.36193(2) 0.129379(9) 0.02240(7) Uani 1 d . . .
Fe2 Fe 0.66243(3) 0.28572(2) 0.244458(9) 0.02325(7) Uani 1 d . . .
S1 S 0.97720(8) 0.15212(5) 0.01961(2) 0.04345(14) Uani 1 d . . .
S2 S 1.04118(7) -0.00847(5) 0.29147(2) 0.04187(14) Uani 1 d . . .
O1 O 0.45017(18) 0.25392(12) 0.13687(5) 0.0328(3) Uani 1 d . . .
O2 O 0.46791(18) 0.19830(11) 0.21342(5) 0.0318(3) Uani 1 d . . .
O3 O 0.78808(16) 0.34629(11) 0.18928(5) 0.0294(3) Uani 1 d . . .
N1 N 0.4593(2) 0.44096(15) 0.08014(6) 0.0317(4) Uani 1 d . . .
N2 N 0.7575(2) 0.50912(14) 0.10984(6) 0.0297(4) Uani 1 d . . .
N3 N 0.4968(2) 0.30076(14) 0.30615(6) 0.0325(4) Uani 1 d . . .
N4 N 0.7865(2) 0.38942(13) 0.29551(6) 0.0298(4) Uani 1 d . . .
N5 N 0.7733(2) 0.26702(14) 0.08150(6) 0.0338(4) Uani 1 d . . .
N6 N 0.8098(2) 0.15231(14) 0.26357(6) 0.0334(4) Uani 1 d . . .
C1 C 0.3184(3) 0.4061(2) 0.06207(8) 0.0409(5) Uani 1 d . . .
H1 H 0.2861 0.3357 0.0713 0.045 Uiso 1 calc R . .
C2 C 0.2123(3) 0.46039(19) 0.03126(8) 0.0407(5) Uani 1 d . . .
H2 H 0.1157 0.4269 0.0172 0.045 Uiso 1 calc R . .
C3 C 0.2496(3) 0.5653(2) 0.02119(8) 0.0438(5) Uani 1 d . . .
H3 H 0.1730 0.6085 0.0026 0.048 Uiso 1 calc R . .
C4 C 0.4008(3) 0.6079(2) 0.03838(9) 0.0434(5) Uani 1 d . . .
H4 H 0.4332 0.6787 0.0299 0.048 Uiso 1 calc R . .
C5 C 0.5009(3) 0.54502(17) 0.06779(8) 0.0352(5) Uani 1 d . . .
C6 C 0.6672(3) 0.58137(19) 0.08842(8) 0.0401(5) Uani 1 d . . .
C7 C 0.9332(3) 0.5228(2) 0.12418(9) 0.0448(6) Uani 1 d . . .
H7A H 0.9640 0.5983 0.1177 0.049 Uiso 1 calc R . .
H7B H 0.9993 0.4770 0.1026 0.049 Uiso 1 calc R . .
C8 C 0.9854(3) 0.4974(2) 0.17630(8) 0.0437(5) Uani 1 d . . .
H8A H 0.9284 0.5478 0.1981 0.048 Uiso 1 calc R . .
H8B H 1.1066 0.5101 0.1807 0.048 Uiso 1 calc R . .
C9 C 0.9484(3) 0.38375(19) 0.19232(8) 0.0387(5) Uani 1 d . . .
H9 H 1.0121 0.3364 0.1702 0.043 Uiso 1 calc R . .
C10 C 1.0311(3) 0.3696(2) 0.24271(8) 0.0441(6) Uani 1 d . . .
H10A H 1.0359 0.2917 0.2500 0.049 Uiso 1 calc R . .
H10B H 1.1473 0.3954 0.2413 0.049 Uiso 1 calc R . .
C11 C 0.9538(3) 0.4235(2) 0.28392(9) 0.0433(5) Uani 1 d . . .
H11A H 1.0271 0.4131 0.3134 0.048 Uiso 1 calc R . .
H11B H 0.9505 0.5016 0.2770 0.048 Uiso 1 calc R . .
C12 C 0.7090(3) 0.4233(2) 0.33211(9) 0.0430(5) Uani 1 d . . .
C13 C 0.5471(3) 0.37345(18) 0.34111(9) 0.0405(5) Uani 1 d . . .
C14 C 0.4550(3) 0.3922(2) 0.38269(8) 0.0416(5) Uani 1 d . . .
H14 H 0.4898 0.4434 0.4067 0.046 Uiso 1 calc R . .
C15 C 0.3093(3) 0.3321(2) 0.38721(9) 0.0423(5) Uani 1 d . . .
H15 H 0.2453 0.3420 0.4153 0.047 Uiso 1 calc R . .
C16 C 0.2560(3) 0.2596(2) 0.35238(8) 0.0428(5) Uani 1 d . . .
H16 H 0.1558 0.2200 0.3554 0.047 Uiso 1 calc R . .
C17 C 0.3581(3) 0.2465(2) 0.31161(8) 0.0414(5) Uani 1 d . . .
H17 H 0.3248 0.1962 0.2870 0.046 Uiso 1 calc R . .
C18 C 0.3994(3) 0.19965(19) 0.17208(8) 0.0403(5) Uani 1 d . . .
C19 C 0.2449(3) 0.1336(2) 0.16310(9) 0.0491(6) Uani 1 d . . .
H19A H 0.2043 0.1429 0.1291 0.054 Uiso 1 calc R . .
H19B H 0.1590 0.1570 0.1852 0.054 Uiso 1 calc R . .
H19C H 0.2706 0.0576 0.1691 0.054 Uiso 1 calc R . .
C20 C 0.7294(4) 0.6917(2) 0.07809(10) 0.0493(6) Uani 1 d . . .
H20A H 0.8387 0.7019 0.0945 0.054 Uiso 1 calc R . .
H20B H 0.6511 0.7449 0.0902 0.054 Uiso 1 calc R . .
H20C H 0.7391 0.7008 0.0427 0.054 Uiso 1 calc R . .
C21 C 0.7646(3) 0.5077(2) 0.36854(9) 0.0486(6) Uani 1 d . . .
H21A H 0.8735 0.5358 0.3598 0.053 Uiso 1 calc R . .
H21B H 0.7733 0.4760 0.4013 0.053 Uiso 1 calc R . .
H21C H 0.6834 0.5664 0.3682 0.053 Uiso 1 calc R . .
C22 C 0.8556(3) 0.22174(19) 0.05475(9) 0.0416(5) Uani 1 d . . .
C23 C 0.9069(3) 0.08584(18) 0.27519(9) 0.0420(5) Uani 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
O3 Fe1 O1 106.08(6) . . ?
O3 Fe1 N5 98.84(6) . . ?
O1 Fe1 N5 95.36(7) . . ?
O3 Fe1 N2 91.84(6) . . ?
O1 Fe1 N2 157.71(6) . . ?
N5 Fe1 N2 94.84(7) . . ?
O3 Fe1 N1 156.07(6) . . ?
O1 Fe1 N1 83.02(6) . . ?
N5 Fe1 N1 102.34(7) . . ?
N2 Fe1 N1 75.47(7) . . ?
O3 Fe2 O2 106.60(6) . . ?
O3 Fe2 N6 100.99(6) . . ?
O2 Fe2 N6 95.58(6) . . ?
O3 Fe2 N4 91.67(6) . . ?
O2 Fe2 N4 157.25(6) . . ?
N6 Fe2 N4 94.06(7) . . ?
O3 Fe2 N3 152.58(6) . . ?
O2 Fe2 N3 83.63(6) . . ?
N6 Fe2 N3 103.26(7) . . ?
N4 Fe2 N3 74.11(7) . . ?
C18 O1 Fe1 133.92(14) . . ?
C18 O2 Fe2 132.27(14) . . ?
C9 O3 Fe2 125.78(13) . . ?
C9 O3 Fe1 123.17(13) . . ?
Fe2 O3 Fe1 110.69(6) . . ?
C1 N1 C5 115.94(19) . . ?
C1 N1 Fe1 129.63(16) . . ?
C5 N1 Fe1 114.41(13) . . ?
C6 N2 C7 124.40(19) . . ?
C6 N2 Fe1 117.78(15) . . ?
C7 N2 Fe1 117.73(14) . . ?
C17 N3 C13 119.32(19) . . ?
C17 N3 Fe2 125.73(15) . . ?
C13 N3 Fe2 114.95(14) . . ?
C12 N4 C11 123.99(19) . . ?
C12 N4 Fe2 119.20(15) . . ?
C11 N4 Fe2 116.65(13) . . ?
C22 N5 Fe1 174.41(19) . . ?
C23 N6 Fe2 172.35(18) . . ?
N1 C1 C2 126.2(2) . . ?
C1 C2 C3 117.6(2) . . ?
C2 C3 C4 119.4(2) . . ?
C5 C4 C3 117.9(2) . . ?
C4 C5 N1 122.6(2) . . ?
C4 C5 C6 123.1(2) . . ?
N1 C5 C6 114.24(18) . . ?
N2 C6 C20 122.9(2) . . ?
N2 C6 C5 116.1(2) . . ?
C20 C6 C5 120.4(2) . . ?
N2 C7 C8 117.5(2) . . ?
C7 C8 C9 114.8(2) . . ?
O3 C9 C8 119.7(2) . . ?
O3 C9 C10 113.20(19) . . ?
C8 C9 C10 106.70(19) . . ?
C11 C10 C9 117.4(2) . . ?
N4 C11 C10 117.01(19) . . ?
N4 C12 C13 117.1(2) . . ?
N4 C12 C21 127.7(2) . . ?
C13 C12 C21 115.3(2) . . ?
N3 C13 C14 121.8(2) . . ?
N3 C13 C12 113.8(2) . . ?
C14 C13 C12 124.3(2) . . ?
C15 C14 C13 116.9(2) . . ?
C16 C15 C14 122.2(2) . . ?
C15 C16 C17 116.5(2) . . ?
N3 C17 C16 123.2(2) . . ?
O2 C18 O1 124.1(2) . . ?
O2 C18 C19 118.5(2) . . ?
O1 C18 C19 117.3(2) . . ?
N5 C22 S1 176.2(2) . . ?
N6 C23 S2 179.3(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
Fe1 O3 1.9998(13) . ?
Fe1 O1 2.0476(14) . ?
Fe1 N5 2.0911(18) . ?
Fe1 N2 2.1402(17) . ?
Fe1 N1 2.1762(17) . ?
Fe2 O3 1.9958(14) . ?
Fe2 O2 2.0614(14) . ?
Fe2 N6 2.0949(18) . ?
Fe2 N4 2.1229(17) . ?
Fe2 N3 2.1972(18) . ?
S1 C22 1.644(3) . ?
S2 C23 1.645(3) . ?
O1 C18 1.257(3) . ?
O2 C18 1.239(3) . ?
O3 C9 1.370(3) . ?
N1 C1 1.294(3) . ?
N1 C5 1.383(3) . ?
N2 C6 1.283(3) . ?
N2 C7 1.461(3) . ?
N3 C17 1.316(3) . ?
N3 C13 1.367(3) . ?
N4 C12 1.272(3) . ?
N4 C11 1.457(3) . ?
N5 C22 1.152(3) . ?
N6 C23 1.173(3) . ?
C1 C2 1.356(3) . ?
C2 C3 1.370(3) . ?
C3 C4 1.391(3) . ?
C4 C5 1.363(3) . ?
C5 C6 1.501(3) . ?
C6 C20 1.492(3) . ?
C7 C8 1.505(3) . ?
C8 C9 1.514(3) . ?
C9 C10 1.518(3) . ?
C10 C11 1.470(3) . ?
C12 C13 1.471(3) . ?
C12 C21 1.504(3) . ?
C13 C14 1.400(3) . ?
C14 C15 1.399(3) . ?
C15 C16 1.370(3) . ?
C16 C17 1.419(3) . ?
C18 C19 1.502(3) . ?
