#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:32:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179145 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/06/4310621.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_4310621
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            'C39 H50 Fe4 N26 O3'
_chemical_formula_weight         1154.45
_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                91.529(15)
_cell_angle_beta                 101.078(16)
_cell_angle_gamma                106.341(14)
_cell_formula_units_Z            1
_cell_length_a                   9.1246(11)
_cell_length_b                   10.2466(11)
_cell_length_c                   14.928(2)
_cell_measurement_temperature    160(2)
_cell_volume                     1309.5(3)
_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      160(2)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_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  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10702
_diffrn_reflns_theta_full        24.09
_diffrn_reflns_theta_max         24.09
_diffrn_reflns_theta_min         2.40
_exptl_absorpt_coefficient_mu    1.149
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Blue-Black
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             594
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.831
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         3920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.831
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0250
_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)+(0.0518P)²+0.1387P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0504
_refine_ls_wR_factor_ref         0.0509
_reflns_number_gt                3231
_reflns_number_total             3920
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0351904si20040114_092725_3.cif
_cod_data_source_block           (4)
_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 'None' changed to
'none' 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^)+(0.0518P)^2^+0.1387P] 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^)+(0.0518P)^2^+0.1387P] 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        1309.6(3)
_cod_database_code               4310621
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
Fe1 Fe 0.450922(16) 0.125355(16) 0.443103(10) 0.02784(6) Uani 1 d . . .
Fe2 Fe 0.396119(17) 0.112101(16) 0.224605(10) 0.03021(6) Uani 1 d . . .
O1 O 0.29946(9) 0.03869(9) 0.33118(5) 0.03688(19) Uani 1 d . . .
N1 N 0.59264(10) 0.28466(10) 0.54439(6) 0.0325(2) Uani 1 d . . .
N2 N 0.29502(10) 0.23137(10) 0.47723(6) 0.0318(2) Uani 1 d . . .
N3 N 0.27862(11) -0.09282(10) 0.16741(6) 0.0359(2) Uani 1 d . . .
N4 N 0.54776(11) 0.05679(10) 0.15004(6) 0.0338(2) Uani 1 d . . .
N5 N 0.56548(11) 0.23718(10) 0.33346(7) 0.0339(2) Uani 1 d . . .
N6 N 0.70997(12) 0.27864(11) 0.34137(7) 0.0398(2) Uani 1 d . . .
N7 N 0.84167(12) 0.31976(11) 0.35167(7) 0.0433(3) Uani 1 d . . .
N8 N 0.62397(10) 0.01553(10) 0.45436(6) 0.0304(2) Uani 1 d . . .
N9 N 0.64851(10) -0.03614(10) 0.38698(7) 0.0340(2) Uani 1 d . . .
N10 N 0.67227(11) -0.08902(11) 0.32449(7) 0.0421(2) Uani 1 d . . .
N11 N 0.31740(12) 0.25443(11) 0.16009(7) 0.0428(3) Uani 1 d . . .
N12 N 0.22570(12) 0.27397(11) 0.10433(8) 0.0437(3) Uani 1 d . . .
N13 N 0.13711(12) 0.29824(12) 0.04616(8) 0.0471(3) Uani 1 d . . .
C1 C 0.74859(14) 0.31485(14) 0.56955(9) 0.0420(3) Uani 1 d . . .
H1 H 0.8002 0.2590 0.5441 0.046 Uiso 1 calc R . .
C2 C 0.83753(15) 0.42567(15) 0.63196(9) 0.0485(3) Uani 1 d . . .
H2 H 0.9477 0.4445 0.6493 0.053 Uiso 1 calc R . .
C3 C 0.76305(14) 0.50609(14) 0.66734(9) 0.0457(3) Uani 1 d . . .
H3 H 0.8211 0.5816 0.7103 0.050 Uiso 1 calc R . .
C4 C 0.60344(14) 0.47812(14) 0.64088(9) 0.0438(3) Uani 1 d . . .
H4 H 0.5517 0.5349 0.6652 0.048 Uiso 1 calc R . .
C5 C 0.51814(14) 0.36724(13) 0.57891(8) 0.0396(3) Uani 1 d . . .
C6 C 0.34693(14) 0.32232(14) 0.54349(9) 0.0420(3) Uani 1 d . . .
C7 C 0.12299(14) 0.17161(14) 0.44511(9) 0.0424(3) Uani 1 d . . .
H7A H 0.0718 0.2435 0.4521 0.047 Uiso 1 calc R . .
H7B H 0.0848 0.0992 0.4848 0.047 Uiso 1 calc R . .
C8 C 0.07430(14) 0.11097(14) 0.34540(9) 0.0435(3) Uani 1 d . . .
H8A H -0.0412 0.0801 0.3287 0.048 Uiso 1 calc R . .
H8B H 0.1108 0.1846 0.3062 0.048 Uiso 1 calc R . .
C9 C 0.13353(14) -0.00689(14) 0.32298(9) 0.0438(3) Uani 1 d . . .
H9 H 0.1082 -0.0772 0.3672 0.048 Uiso 1 calc R . .
C10 C 0.05501(14) -0.07057(14) 0.22710(9) 0.0465(3) Uani 1 d . . .
H10A H 0.0523 0.0038 0.1864 0.051 Uiso 1 calc R . .
H10B H -0.0545 -0.1218 0.2274 0.051 Uiso 1 calc R . .
C11 C 0.13008(14) -0.16687(14) 0.18580(9) 0.0470(3) Uani 1 d . . .
H11A H 0.1444 -0.2362 0.2289 0.052 Uiso 1 calc R . .
H11B H 0.0601 -0.2149 0.1281 0.052 Uiso 1 calc R . .
C12 C 0.35709(15) -0.15782(14) 0.13297(9) 0.0443(3) Uani 1 d . . .
C13 C 0.50834(14) -0.07325(14) 0.11698(9) 0.0428(3) Uani 1 d . . .
C14 C 0.60511(15) -0.11886(15) 0.06848(9) 0.0437(3) Uani 1 d . . .
H14 H 0.5772 -0.2117 0.0453 0.048 Uiso 1 calc R . .
C15 C 0.74111(14) -0.02734(14) 0.05491(9) 0.0422(3) Uani 1 d . . .
H15 H 0.8061 -0.0574 0.0215 0.046 Uiso 1 calc R . .
C16 C 0.78282(14) 0.10576(14) 0.08901(8) 0.0419(3) Uani 1 d . . .
H16 H 0.8763 0.1689 0.0800 0.046 Uiso 1 calc R . .
C17 C 0.68472(14) 0.14708(14) 0.13757(8) 0.0421(3) Uani 1 d . . .
H17 H 0.7130 0.2392 0.1625 0.046 Uiso 1 calc R . .
C18 C 0.25147(15) 0.38746(15) 0.59278(9) 0.0461(3) Uani 1 d . . .
H18A H 0.1406 0.3502 0.5641 0.051 Uiso 1 calc R . .
H18B H 0.2843 0.4864 0.5889 0.051 Uiso 1 calc R . .
H18C H 0.2677 0.3679 0.6572 0.051 Uiso 1 calc R . .
C19 C 0.30932(15) -0.31035(14) 0.10881(9) 0.0483(3) Uani 1 d . . .
H19A H 0.2080 -0.3524 0.1245 0.053 Uiso 1 calc R . .
H19B H 0.3878 -0.3488 0.1433 0.053 Uiso 1 calc R . .
H19C H 0.3013 -0.3287 0.0430 0.053 Uiso 1 calc R . .
O2 O 0.2942(2) 0.4663(2) 0.84795(13) 0.0543(5) Uani 0.50 d P . .
H2A H 0.2084 0.4405 0.8645 0.060 Uiso 0.50 calc PR . .
C20 C 0.4095(3) 0.5384(3) 0.9213(2) 0.0582(7) Uani 0.50 d P . .
H20A H 0.4030 0.6318 0.9286 0.064 Uiso 0.50 calc PR . .
H20B H 0.5123 0.5409 0.9097 0.064 Uiso 0.50 calc PR . .
H20C H 0.3945 0.4935 0.9774 0.064 Uiso 0.50 calc PR . .
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'
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
O1 Fe1 N1 158.26(4) . . ?
O1 Fe1 N2 90.60(4) . . ?
N1 Fe1 N2 74.99(4) . . ?
O1 Fe1 N8 103.65(4) . . ?
N1 Fe1 N8 93.96(4) . . ?
N2 Fe1 N8 162.11(4) . . ?
O1 Fe1 N8 102.10(4) . 2_656 ?
N1 Fe1 N8 93.37(4) . 2_656 ?
N2 Fe1 N8 86.65(4) . 2_656 ?
N8 Fe1 N8 79.90(4) . 2_656 ?
O1 Fe1 N5 78.43(4) . . ?
N1 Fe1 N5 90.26(4) . . ?
N2 Fe1 N5 107.40(4) . . ?
N8 Fe1 N5 86.31(4) . . ?
N8 Fe1 N5 165.95(3) 2_656 . ?
N11 Fe2 O1 116.65(4) . . ?
N11 Fe2 N4 107.96(4) . . ?
O1 Fe2 N4 134.86(4) . . ?
N11 Fe2 N5 99.57(4) . . ?
O1 Fe2 N5 80.81(4) . . ?
N4 Fe2 N5 98.84(4) . . ?
N11 Fe2 N3 114.86(4) . . ?
O1 Fe2 N3 81.06(4) . . ?
N4 Fe2 N3 74.28(4) . . ?
N5 Fe2 N3 145.42(4) . . ?
C9 O1 Fe1 125.02(7) . . ?
C9 O1 Fe2 121.45(7) . . ?
Fe1 O1 Fe2 106.71(4) . . ?
C1 N1 C5 119.14(10) . . ?
C1 N1 Fe1 124.23(8) . . ?
C5 N1 Fe1 116.37(8) . . ?
C6 N2 C7 119.45(10) . . ?
C6 N2 Fe1 117.63(8) . . ?
C7 N2 Fe1 120.15(8) . . ?
C12 N3 C11 119.01(12) . . ?
C12 N3 Fe2 117.64(9) . . ?
C11 N3 Fe2 121.71(8) . . ?
C13 N4 C17 119.95(11) . . ?
C13 N4 Fe2 116.91(8) . . ?
C17 N4 Fe2 123.10(9) . . ?
N6 N5 Fe2 128.53(8) . . ?
N6 N5 Fe1 122.61(8) . . ?
Fe2 N5 Fe1 93.40(4) . . ?
N7 N6 N5 177.14(12) . . ?
N9 N8 Fe1 121.12(7) . . ?
N9 N8 Fe1 115.62(8) . 2_656 ?
Fe1 N8 Fe1 100.10(4) . 2_656 ?
N10 N9 N8 177.69(12) . . ?
N12 N11 Fe2 145.37(10) . . ?
N11 N12 N13 177.00(13) . . ?
N1 C1 C2 122.17(12) . . ?
N1 C1 H1 118.9 . . ?
C2 C1 H1 118.9 . . ?
C3 C2 C1 118.56(12) . . ?
C3 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
C2 C3 C4 120.00(13) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C3 C4 C5 120.16(13) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
N1 C5 C4 119.94(11) . . ?
N1 C5 C6 112.81(11) . . ?
C4 C5 C6 127.25(12) . . ?
N2 C6 C5 117.05(11) . . ?
N2 C6 C18 126.59(11) . . ?
C5 C6 C18 116.34(12) . . ?
N2 C7 C8 113.75(10) . . ?
N2 C7 H7A 108.8 . . ?
C8 C7 H7A 108.8 . . ?
N2 C7 H7B 108.8 . . ?
C8 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
C9 C8 C7 116.34(11) . . ?
C9 C8 H8A 108.2 . . ?
C7 C8 H8A 108.2 . . ?
C9 C8 H8B 108.2 . . ?
C7 C8 H8B 108.2 . . ?
H8A C8 H8B 107.4 . . ?
O1 C9 C8 110.27(10) . . ?
O1 C9 C10 109.99(11) . . ?
C8 C9 C10 110.18(11) . . ?
O1 C9 H9 108.8 . . ?
C8 C9 H9 108.8 . . ?
C10 C9 H9 108.8 . . ?
C9 C10 C11 116.17(11) . . ?
C9 C10 H10A 108.2 . . ?
C11 C10 H10A 108.2 . . ?
C9 C10 H10B 108.2 . . ?
C11 C10 H10B 108.2 . . ?
H10A C10 H10B 107.4 . . ?
N3 C11 C10 110.85(11) . . ?
N3 C11 H11A 109.5 . . ?
C10 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 108.1 . . ?
N3 C12 C13 115.09(12) . . ?
N3 C12 C19 125.89(12) . . ?
C13 C12 C19 119.01(12) . . ?
N4 C13 C14 120.36(12) . . ?
N4 C13 C12 114.36(12) . . ?
C14 C13 C12 125.25(13) . . ?
C15 C14 C13 119.44(13) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C16 C15 C14 120.58(13) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C15 C16 C17 118.40(12) . . ?
C15 C16 H16 120.8 . . ?
C17 C16 H16 120.8 . . ?
N4 C17 C16 121.26(12) . . ?
N4 C17 H17 119.4 . . ?
C16 C17 H17 119.4 . . ?
C6 C18 H18A 109.5 . . ?
C6 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C6 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C12 C19 H19A 109.5 . . ?
C12 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C12 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C20 O2 H2A 109.5 . . ?
O2 C20 H20A 109.5 . . ?
O2 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O2 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
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 O1 1.9578(9) . ?
Fe1 N1 2.1336(11) . ?
Fe1 N2 2.1405(9) . ?
Fe1 N8 2.1669(9) . ?
Fe1 N8 2.2043(10) 2_656 ?
Fe1 N5 2.2733(11) . ?
Fe2 N11 1.9922(11) . ?
Fe2 O1 2.0261(9) . ?
Fe2 N4 2.1152(10) . ?
Fe2 N5 2.1168(11) . ?
Fe2 N3 2.1385(11) . ?
O1 C9 1.4328(15) . ?
N1 C1 1.3425(15) . ?
N1 C5 1.3706(16) . ?
N2 C6 1.2623(17) . ?
N2 C7 1.4910(15) . ?
N3 C12 1.2697(17) . ?
N3 C11 1.4365(16) . ?
N4 C13 1.3325(17) . ?
N4 C17 1.3786(16) . ?
N5 N6 1.2470(14) . ?
N6 N7 1.1340(14) . ?
N8 N9 1.2113(13) . ?
N8 Fe1 2.2043(10) 2_656 ?
N9 N10 1.1523(14) . ?
N11 N12 1.1263(15) . ?
N12 N13 1.1508(15) . ?
C1 C2 1.3965(19) . ?
C1 H1 0.9500 . ?
C2 C3 1.360(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.3774(18) . ?
C3 H3 0.9500 . ?
C4 C5 1.3863(19) . ?
C4 H4 0.9500 . ?
C5 C6 1.4823(17) . ?
C6 C18 1.5143(18) . ?
C7 C8 1.5298(18) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.5094(19) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.5102(17) . ?
C9 H9 1.0000 . ?
C10 C11 1.5275(19) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.4756(19) . ?
C12 C19 1.513(2) . ?
C13 C14 1.4078(19) . ?
C14 C15 1.3829(18) . ?
C14 H14 0.9500 . ?
C15 C16 1.3640(19) . ?
C15 H15 0.9500 . ?
C16 C17 1.3973(18) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
O2 C20 1.389(3) . ?
O2 H2A 0.8400 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
