#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:26:17 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179377 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/74/4327498.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_4327498
loop_
_publ_author_name
'Juan M. Clemente-Juan'
'Christine Mackiewicz'
'Marc Verelst'
'Françoise Dahan'
'Azzedine Bousseksou'
'Yiannis Sanakis'
'Jean-Pierre Tuchagues'
_publ_contact_author
;
         Prof. Jean-Pierre Tuchagues
         Laboratoire de Chimie de Coordination du CNRS
         205 Route de Narbonne
         31077 Toulouse Cedex 4
         France
;
_publ_contact_author_email       tuchague@lcc-toulouse.fr
_publ_contact_author_fax         '(33) 0561553003'
_publ_contact_author_phone       '(33) 0561333154'
_publ_section_title
;
 Synthesis, Structure, and Magnetic Properties of Tetranuclear Cubane-like
 and Chain-like Iron(II) Complexes Based on the N4O Pentadentate
 Dinucleating Ligand 1,5-Bis[(2-pyridylmethyl)amino]pentan-3-ol
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1478
_journal_page_last               1491
_journal_paper_doi               10.1021/ic010787+
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C40 H46 Fe4 N14 O8'
_chemical_formula_weight         1074.31
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 99.359(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.7633(18)
_cell_length_b                   18.234(3)
_cell_length_c                   10.4792(16)
_cell_measurement_temperature    160(2)
_cell_volume                     2217.8(6)
_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      160(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0595
_diffrn_reflns_av_sigmaI/netI    0.0482
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17070
_diffrn_reflns_theta_full        26.13
_diffrn_reflns_theta_max         26.13
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    1.351
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Oranged-Yellow
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4335
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.921
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0346
_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)+(0.0434P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0803
_reflns_number_gt                3030
_reflns_number_total             4335
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0107872B_3.cif
_cod_data_source_block           (3)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0434P)^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^)+(0.0434P)^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        2217.7(6)
_cod_database_code               4327498
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, 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
Fe1 Fe 0.53628(3) 0.06359(2) 0.89088(4) 0.02799(11) Uani 1 d .
Fe2 Fe 0.77438(3) 0.02993(2) 0.79686(4) 0.03269(12) Uani 1 d .
O1 O 0.69444(16) 0.10871(10) 0.87557(18) 0.0327(4) Uani 1 d .
O2 O 0.18701(19) 0.00041(17) 0.8839(3) 0.0696(8) Uani 1 d .
O3 O 0.93102(19) -0.17788(13) 0.7451(2) 0.0505(6) Uani 1 d .
O4 O 0.5479(2) -0.14081(12) 0.7323(2) 0.0536(6) Uani 1 d .
N1 N 0.41331(19) 0.11550(13) 0.7372(2) 0.0326(5) Uani 1 d .
N2 N 0.4816(2) 0.16242(14) 0.9829(2) 0.0406(6) Uani 1 d .
H2A H 0.4807 0.1513 1.0694 0.045 Uiso 1 calc R
N3 N 0.9463(2) 0.08070(15) 0.8284(2) 0.0413(6) Uani 1 d .
H3A H 0.9920 0.0555 0.8950 0.045 Uiso 1 calc R
N4 N 0.79280(19) 0.06810(13) 0.6073(2) 0.0350(5) Uani 1 d .
N5 N 0.3904(2) -0.00240(14) 0.9273(2) 0.0355(5) Uani 1 d .
N6 N 0.8495(2) -0.06988(16) 0.8169(3) 0.0500(7) Uani 1 d .
N7 N 0.59957(19) -0.01518(13) 0.7580(2) 0.0350(5) Uani 1 d .
C1 C 0.3923(2) 0.09604(17) 0.6123(3) 0.0355(6) Uani 1 d .
H1 H 0.4419 0.0613 0.5820 0.039 Uiso 1 calc R
C2 C 0.3022(2) 0.12404(19) 0.5259(3) 0.0440(8) Uani 1 d .
H2 H 0.2886 0.1082 0.4384 0.048 Uiso 1 calc R
C3 C 0.2323(3) 0.17556(19) 0.5696(3) 0.0479(8) Uani 1 d .
H3 H 0.1705 0.1968 0.5118 0.053 Uiso 1 calc R
C4 C 0.2523(3) 0.19599(17) 0.6968(3) 0.0446(8) Uani 1 d .
H4 H 0.2049 0.2317 0.7280 0.049 Uiso 1 calc R
C5 C 0.3425(2) 0.16395(16) 0.7796(3) 0.0371(7) Uani 1 d .
C6 C 0.3622(3) 0.17949(19) 0.9230(3) 0.0479(8) Uani 1 d .
H6A H 0.3461 0.2319 0.9375 0.053 Uiso 1 calc R
H6B H 0.3082 0.1497 0.9648 0.053 Uiso 1 calc R
C7 C 0.5572(3) 0.22670(17) 0.9793(3) 0.0492(8) Uani 1 d .
H7A H 0.5331 0.2659 1.0346 0.054 Uiso 1 calc R
H7B H 0.5479 0.2456 0.8896 0.054 Uiso 1 calc R
C8 C 0.6821(3) 0.20893(18) 1.0248(3) 0.0470(8) Uani 1 d .
H8A H 0.6874 0.1735 1.0971 0.052 Uiso 1 calc R
H8B H 0.7224 0.2543 1.0588 0.052 Uiso 1 calc R
C9 C 0.7435(3) 0.17723(16) 0.9214(3) 0.0376(7) Uani 1 d .
H9 H 0.7316 0.2121 0.8467 0.041 Uiso 1 calc R
C10 C 0.8730(3) 0.17200(19) 0.9680(3) 0.0486(8) Uani 1 d .
H10A H 0.8990 0.2182 1.0133 0.053 Uiso 1 calc R
H10B H 0.8874 0.1318 1.0321 0.053 Uiso 1 calc R
C11 C 0.9452(3) 0.15875(19) 0.8647(3) 0.0491(8) Uani 1 d .
H11A H 0.9145 0.1882 0.7874 0.054 Uiso 1 calc R
H11B H 1.0251 0.1752 0.8961 0.054 Uiso 1 calc R
C12 C 0.9934(3) 0.0681(2) 0.7086(3) 0.0454(8) Uani 1 d .
H12A H 1.0209 0.0169 0.7065 0.050 Uiso 1 calc R
H12B H 1.0598 0.1012 0.7062 0.050 Uiso 1 calc R
C13 C 0.9023(2) 0.08227(17) 0.5925(3) 0.0388(7) Uani 1 d .
C14 C 0.9274(3) 0.1054(2) 0.4749(3) 0.0466(8) Uani 1 d .
H14 H 1.0050 0.1148 0.4654 0.051 Uiso 1 calc R
C15 C 0.8409(3) 0.1147(2) 0.3717(3) 0.0481(8) Uani 1 d .
H15 H 0.8580 0.1304 0.2905 0.053 Uiso 1 calc R
C16 C 0.7295(3) 0.1010(2) 0.3871(3) 0.0464(8) Uani 1 d .
H16 H 0.6679 0.1073 0.3171 0.051 Uiso 1 calc R
C17 C 0.7088(2) 0.07804(17) 0.5060(3) 0.0386(7) Uani 1 d .
H17 H 0.6315 0.0688 0.5169 0.042 Uiso 1 calc R
C18 C 0.2888(2) -0.00039(17) 0.9047(3) 0.0357(6) Uani 1 d .
C19 C 0.8901(2) -0.12349(18) 0.7816(3) 0.0355(7) Uani 1 d .
C20 C 0.5742(2) -0.07753(16) 0.7445(3) 0.0331(6) 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'
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_3
O1 Fe1 N5 168.18(8) .
O1 Fe1 N2 92.26(9) .
N5 Fe1 N2 94.64(10) .
O1 Fe1 N1 105.41(8) .
N5 Fe1 N1 85.58(9) .
N2 Fe1 N1 76.28(9) .
O1 Fe1 N7 79.05(8) .
N5 Fe1 N7 96.14(9) .
N2 Fe1 N7 164.76(9) .
N1 Fe1 N7 93.85(9) .
O1 Fe1 N5 92.12(8) 3_657
N5 Fe1 N5 77.46(10) 3_657
N2 Fe1 N5 97.73(9) 3_657
N1 Fe1 N5 161.56(8) 3_657
N7 Fe1 N5 95.10(9) 3_657
O1 Fe2 N6 147.62(10) .
O1 Fe2 N4 106.12(9) .
N6 Fe2 N4 106.24(11) .
O1 Fe2 N7 81.61(8) .
N6 Fe2 N7 93.59(10) .
N4 Fe2 N7 100.51(9) .
O1 Fe2 N3 96.89(9) .
N6 Fe2 N3 89.28(10) .
N4 Fe2 N3 76.95(9) .
N7 Fe2 N3 176.62(9) .
C9 O1 Fe2 125.83(17) .
C9 O1 Fe1 130.03(17) .
Fe2 O1 Fe1 103.86(8) .
C5 N1 C1 118.2(2) .
C5 N1 Fe1 114.32(18) .
C1 N1 Fe1 126.67(19) .
C6 N2 C7 110.9(3) .
C6 N2 Fe1 108.29(18) .
C7 N2 Fe1 114.89(19) .
C12 N3 C11 113.0(2) .
C12 N3 Fe2 105.73(18) .
C11 N3 Fe2 113.51(18) .
C17 N4 C13 118.6(2) .
C17 N4 Fe2 127.15(18) .
C13 N4 Fe2 114.23(19) .
C18 N5 Fe1 138.4(2) .
C18 N5 Fe1 114.9(2) 3_657
Fe1 N5 Fe1 102.54(10) 3_657
C19 N6 Fe2 155.7(3) .
C20 N7 Fe2 126.6(2) .
C20 N7 Fe1 126.7(2) .
Fe2 N7 Fe1 92.35(9) .
N1 C1 C2 123.0(3) .
C3 C2 C1 118.2(3) .
C4 C3 C2 119.6(3) .
C3 C4 C5 119.2(3) .
N1 C5 C4 121.6(3) .
N1 C5 C6 116.8(2) .
C4 C5 C6 121.5(3) .
N2 C6 C5 111.4(2) .
N2 C7 C8 112.5(3) .
C7 C8 C9 114.3(3) .
O1 C9 C8 111.2(2) .
O1 C9 C10 112.4(2) .
C8 C9 C10 111.3(2) .
C11 C10 C9 115.6(3) .
N3 C11 C10 111.8(3) .
N3 C12 C13 110.2(2) .
N4 C13 C14 120.6(3) .
N4 C13 C12 116.3(2) .
C14 C13 C12 123.1(3) .
C15 C14 C13 120.2(3) .
C16 C15 C14 119.2(3) .
C15 C16 C17 118.5(3) .
N4 C17 C16 122.9(3) .
N5 C18 O2 178.5(3) .
N6 C19 O3 179.6(3) .
N7 C20 O4 179.1(3) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O1 2.0642(18) .
Fe1 N5 2.180(2) .
Fe1 N2 2.189(2) .
Fe1 N1 2.197(2) .
Fe1 N7 2.212(2) .
Fe1 N5 2.255(2) 3_657
Fe2 O1 1.9698(19) .
Fe2 N6 2.019(3) .
Fe2 N4 2.149(2) .
Fe2 N7 2.191(2) .
Fe2 N3 2.200(2) .
O1 C9 1.426(3) .
O2 C18 1.182(3) .
O3 C19 1.192(4) .
O4 C20 1.196(4) .
N1 C5 1.338(4) .
N1 C1 1.340(3) .
N2 C6 1.475(4) .
N2 C7 1.475(4) .
N3 C12 1.471(4) .
N3 C11 1.473(4) .
N4 C17 1.340(4) .
N4 C13 1.347(3) .
N5 C18 1.180(3) .
N5 Fe1 2.255(2) 3_657
N6 C19 1.174(4) .
N7 C20 1.178(4) .
C1 C2 1.375(4) .
C2 C3 1.375(5) .
C3 C4 1.367(5) .
C4 C5 1.386(4) .
C5 C6 1.510(4) .
C7 C8 1.504(5) .
C8 C9 1.512(4) .
C9 C10 1.526(4) .
C10 C11 1.501(5) .
C12 C13 1.507(4) .
C13 C14 1.379(4) .
C14 C15 1.370(5) .
C15 C16 1.369(4) .
C16 C17 1.373(4) .
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
N2 H2A O4 0.93 2.17 3.085(3) 168.9 3_657
N3 H3A O2 0.93 2.52 3.157(3) 125.6 1_655
