#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:32:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179145 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/06/4310622.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_4310622
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            'C21 H26 Fe N6 O2 S2'
_chemical_formula_weight         514.45
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                106.685(14)
_cell_angle_beta                 93.689(14)
_cell_angle_gamma                108.508(13)
_cell_formula_units_Z            2
_cell_length_a                   8.7674(9)
_cell_length_b                   12.0938(13)
_cell_length_c                   12.2634(14)
_cell_measurement_temperature    180(2)
_cell_volume                     1163.7(3)
_computing_cell_refinement       'STOE-IPDS software (Stoe, 2.87, 1997)'
_computing_data_collection       'STOE-IPDS software (Stoe, 2.87, 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 0.922
_diffrn_measured_fraction_theta_max 0.922
_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  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11514
_diffrn_reflns_theta_full        26.13
_diffrn_reflns_theta_max         26.13
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.858
_exptl_absorpt_correction_T_max  0.6909
_exptl_absorpt_correction_T_min  0.3778
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-SHAPE (Stoe & Cie, 1996)'
_exptl_crystal_colour            Blue-Black
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4259
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0904P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.0932
_reflns_number_gt                3357
_reflns_number_total             4259
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0351904si20040114_092725_4.cif
_cod_data_source_block           (8)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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^)+(0.0904P)^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^)+(0.0904P)^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_original_cell_volume        1163.7(2)
_cod_database_code               4310622
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Fe Fe 0.22788(3) 0.15801(3) 0.29465(2) 0.02953(12) Uani 1 d . . .
S1 S -0.33701(7) -0.03402(7) 0.29140(5) 0.04861(18) Uani 1 d . . .
S2 S 0.00743(8) 0.45281(6) 0.24968(6) 0.04789(17) Uani 1 d . . .
N1 N 0.25650(19) 0.00839(16) 0.30183(14) 0.0301(3) Uani 1 d . . .
N2 N 0.2141(2) 0.07652(16) 0.12966(14) 0.0310(4) Uani 1 d . . .
N3 N 0.2630(2) 0.23875(17) 0.46178(15) 0.0331(4) Uani 1 d . . .
N4 N 0.4596(2) 0.24592(16) 0.32031(13) 0.0287(3) Uani 1 d . . .
N5 N -0.0063(2) 0.07438(18) 0.28504(15) 0.0347(4) Uani 1 d . . .
N6 N 0.1747(2) 0.29708(17) 0.27400(15) 0.0349(4) Uani 1 d . . .
C1 C 0.2876(3) -0.0211(2) 0.39672(19) 0.0375(5) Uani 1 d . . .
H1 H 0.3094 0.0403 0.4701 0.041 Uiso 1 calc R . .
C2 C 0.2896(3) -0.1340(2) 0.3932(2) 0.0475(6) Uani 1 d . . .
H2 H 0.3123 -0.1503 0.4627 0.052 Uiso 1 calc R . .
C3 C 0.2579(3) -0.2256(2) 0.2863(3) 0.0513(6) Uani 1 d . . .
H3 H 0.2571 -0.3056 0.2814 0.056 Uiso 1 calc R . .
C4 C 0.2274(3) -0.1968(2) 0.1874(2) 0.0457(5) Uani 1 d . . .
H4 H 0.2076 -0.2569 0.1134 0.050 Uiso 1 calc R . .
C5 C 0.2260(2) -0.0816(2) 0.19657(19) 0.0339(4) Uani 1 d . . .
C6 C 0.2048(2) -0.0384(2) 0.09922(17) 0.0317(4) Uani 1 d . . .
C7 C 0.2205(3) 0.1388(2) 0.04321(18) 0.0374(5) Uani 1 d . . .
H7A H 0.1738 0.2046 0.0683 0.041 Uiso 1 calc R . .
H7B H 0.1537 0.0789 -0.0311 0.041 Uiso 1 calc R . .
C8 C 0.3955(3) 0.1948(2) 0.0258(2) 0.0434(5) Uani 1 d . . .
O1A O 0.4089(4) 0.2541(3) -0.0573(3) 0.0497(8) Uani 0.50 d P A 1
H1A H 0.3249 0.2701 -0.0686 0.054 Uiso 0.50 calc PR A 1
H8A H 0.4381 0.1258 -0.0013 0.048 Uiso 0.50 d P B 1
O1B O 0.4594(4) 0.1068(4) -0.0252(3) 0.0485(8) Uani 0.50 d P A 2
H1B H 0.4382 0.0524 0.0061 0.053 Uiso 0.50 calc PR A 2
H8B H 0.3913 0.2411 -0.0293 0.048 Uiso 0.50 d P C 2
C9 C 0.5113(3) 0.2883(2) 0.13622(19) 0.0437(5) Uani 1 d . . .
H9A H 0.4596 0.3481 0.1730 0.048 Uiso 1 calc R . .
H9B H 0.6128 0.3345 0.1142 0.048 Uiso 1 calc R . .
C10 C 0.5571(3) 0.2325(2) 0.22616(17) 0.0364(5) Uani 1 d . . .
H10A H 0.5377 0.1440 0.1879 0.040 Uiso 1 calc R . .
H10B H 0.6747 0.2745 0.2591 0.040 Uiso 1 calc R . .
C11 C 0.1522(3) 0.2296(2) 0.53295(19) 0.0436(5) Uani 1 d . . .
H11 H 0.0428 0.1760 0.5017 0.048 Uiso 1 calc R . .
C12 C 0.1918(3) 0.2952(2) 0.6496(2) 0.0452(5) Uani 1 d . . .
H12 H 0.1097 0.2879 0.6968 0.050 Uiso 1 calc R . .
C13 C 0.3508(3) 0.3713(3) 0.6977(2) 0.0494(6) Uani 1 d . . .
H13 H 0.3809 0.4138 0.7785 0.054 Uiso 1 calc R . .
C14 C 0.4655(3) 0.3840(2) 0.62534(19) 0.0440(5) Uani 1 d . . .
H14 H 0.5750 0.4381 0.6553 0.048 Uiso 1 calc R . .
C15 C 0.4188(3) 0.31691(19) 0.50886(16) 0.0341(4) Uani 1 d . . .
C16 C 0.5306(3) 0.3182(2) 0.42410(18) 0.0342(4) Uani 1 d . . .
C17 C 0.1820(3) -0.1228(2) -0.0215(2) 0.0464(6) Uani 1 d . . .
H17A H 0.1699 -0.0798 -0.0763 0.051 Uiso 1 calc R . .
H17B H 0.0839 -0.1959 -0.0359 0.051 Uiso 1 calc R . .
H17C H 0.2773 -0.1481 -0.0314 0.051 Uiso 1 calc R . .
C18 C 0.7089(3) 0.3972(3) 0.4623(2) 0.0509(6) Uani 1 d . . .
H18A H 0.7654 0.3872 0.3957 0.056 Uiso 1 calc R . .
H18B H 0.7576 0.3718 0.5207 0.056 Uiso 1 calc R . .
H18C H 0.7196 0.4838 0.4954 0.056 Uiso 1 calc R . .
C19 C -0.1444(3) 0.0280(2) 0.28645(17) 0.0346(4) Uani 1 d . . .
C20 C 0.1054(3) 0.3622(2) 0.26423(17) 0.0370(5) Uani 1 d . . .
C21 C 0.3637(7) 0.5010(4) 0.0337(4) 0.1164(19) Uani 1 d . . .
H21A H 0.3926 0.5907 0.0622 0.128 Uiso 1 calc R . .
H21B H 0.4314 0.4793 -0.0235 0.128 Uiso 1 calc R . .
H21C H 0.3825 0.4719 0.0984 0.128 Uiso 1 calc R . .
O2 O 0.2073(3) 0.4482(3) -0.0150(2) 0.0831(7) Uani 1 d . . .
H2A H 0.1496 0.4433 0.0355 0.092 Uiso 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'
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
N4 Fe N1 92.83(7) . . ?
N4 Fe N2 94.25(7) . . ?
N1 Fe N2 80.99(7) . . ?
N4 Fe N3 81.05(7) . . ?
N1 Fe N3 96.16(8) . . ?
N2 Fe N3 174.41(7) . . ?
N4 Fe N5 174.38(7) . . ?
N1 Fe N5 87.21(7) . . ?
N2 Fe N5 91.30(7) . . ?
N3 Fe N5 93.36(7) . . ?
N4 Fe N6 93.01(7) . . ?
N1 Fe N6 173.10(7) . . ?
N2 Fe N6 94.90(7) . . ?
N3 Fe N6 88.39(8) . . ?
N5 Fe N6 87.33(8) . . ?
C1 N1 C5 117.3(2) . . ?
C1 N1 Fe 127.86(15) . . ?
C5 N1 Fe 114.53(14) . . ?
C6 N2 C7 120.14(18) . . ?
C6 N2 Fe 116.25(14) . . ?
C7 N2 Fe 123.55(14) . . ?
C11 N3 C15 117.48(19) . . ?
C11 N3 Fe 128.08(16) . . ?
C15 N3 Fe 114.39(13) . . ?
C16 N4 C10 119.90(17) . . ?
C16 N4 Fe 118.00(14) . . ?
C10 N4 Fe 122.10(13) . . ?
C19 N5 Fe 175.89(17) . . ?
C20 N6 Fe 163.17(18) . . ?
N1 C1 C2 123.6(2) . . ?
C1 C2 C3 119.1(2) . . ?
C4 C3 C2 118.3(2) . . ?
C5 C4 C3 119.9(2) . . ?
C4 C5 N1 121.8(2) . . ?
C4 C5 C6 124.9(2) . . ?
N1 C5 C6 113.18(19) . . ?
N2 C6 C5 113.69(18) . . ?
N2 C6 C17 126.5(2) . . ?
C5 C6 C17 119.8(2) . . ?
N2 C7 C8 111.07(17) . . ?
O1B C8 O1A 98.7(3) . . ?
O1B C8 C7 112.4(2) . . ?
O1A C8 C7 113.6(2) . . ?
O1B C8 C9 110.3(2) . . ?
O1A C8 C9 106.7(2) . . ?
C7 C8 C9 114.00(19) . . ?
C8 C9 C10 115.2(2) . . ?
N4 C10 C9 111.05(17) . . ?
N3 C11 C12 122.5(2) . . ?
C13 C12 C11 119.9(2) . . ?
C12 C13 C14 118.3(2) . . ?
C15 C14 C13 119.3(2) . . ?
N3 C15 C14 122.5(2) . . ?
N3 C15 C16 113.08(17) . . ?
C14 C15 C16 124.4(2) . . ?
N4 C16 C15 113.32(18) . . ?
N4 C16 C18 126.6(2) . . ?
C15 C16 C18 120.04(19) . . ?
N5 C19 S1 178.57(19) . . ?
N6 C20 S2 179.6(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
Fe N4 1.9266(17) . ?
Fe N1 1.9293(18) . ?
Fe N2 1.9565(17) . ?
Fe N3 1.9565(17) . ?
Fe N5 1.9583(19) . ?
Fe N6 1.9587(19) . ?
S1 C19 1.629(2) . ?
S2 C20 1.632(3) . ?
N1 C1 1.347(3) . ?
N1 C5 1.373(3) . ?
N2 C6 1.305(3) . ?
N2 C7 1.460(3) . ?
N3 C11 1.346(3) . ?
N3 C15 1.363(3) . ?
N4 C16 1.298(3) . ?
N4 C10 1.482(2) . ?
N5 C19 1.165(3) . ?
N6 C20 1.163(3) . ?
C1 C2 1.359(4) . ?
C2 C3 1.395(4) . ?
C3 C4 1.387(4) . ?
C4 C5 1.369(3) . ?
C5 C6 1.457(3) . ?
C6 C17 1.496(3) . ?
C7 C8 1.525(3) . ?
C8 O1B 1.371(4) . ?
C8 O1A 1.397(4) . ?
C8 C9 1.535(3) . ?
C9 C10 1.541(3) . ?
C11 C12 1.381(3) . ?
C12 C13 1.381(4) . ?
C13 C14 1.385(4) . ?
C14 C15 1.384(3) . ?
C15 C16 1.474(3) . ?
C16 C18 1.509(3) . ?
C21 O2 1.328(5) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1A H1A O2 0.84 2.60 3.306(5) 142.4 .
O1B H1B O1B 0.84 2.43 3.111(8) 138.1 2_655
O2 H2A S2 0.84 2.97 3.793(3) 168.1 .
