#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/01/4320153.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_4320153
loop_
_publ_author_name
'Dominique Mandon'
'Agathe Nopper'
'Thomas Litrol'
'Sandrine Goetz'
_publ_contact_author
;
Dr Dominique MANDON
Laboratoire de Chimie Organométallique et de Catalyse
Institut Le bel
4, rue Blaise Pascal
F-67070 Strasbourg Cedex
France
;
_publ_contact_author_email       mandon@chimie.u-strasbg.fr
_publ_contact_author_fax         '+ 33 (0) 390 245 001'
_publ_contact_author_phone       '+ 33 (0) 390 241 537'
_publ_section_title
;
 Tridentate Coordination of Monosubstituted Derivatives of the
 Tris(2-pyridylmethyl)amine Ligand to FeCl3: Structures and Spectroscopic
 Properties of ((2-Bromopyridyl)methyl)bis- (2-pyridylmethyl)amine
 FeIIICl3 and (((2-p- Methoxyphenyl)pyridyl)methyl)Bis(2-pyridyl-
 methyl)]amine FeIIICl3 and Comparison with the Bis(2-pyridylmethyl)]amine
 FeIIICl3 Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4803
_journal_page_last               4806
_journal_paper_doi               10.1021/ic001339p
_journal_volume                  40
_journal_year                    2001
_chemical_formula_analytical     L2Fe(III)Cl3
_chemical_formula_moiety         'C25 H24 N4 O Cl3 Fe'
_chemical_formula_structural     L2Fe(III)Cl3
_chemical_formula_sum            'C25 H24 Cl3 Fe N4 O'
_chemical_formula_weight         558.70
_chemical_name_common            L2Fe(III)Cl3
_chemical_name_systematic        ' L2Fe(III)Cl3'
_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'
_cell_angle_alpha                90
_cell_angle_beta                 109.39(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.9206(6)
_cell_length_b                   7.9500(2)
_cell_length_c                   15.2009(4)
_cell_measurement_reflns_used    22038
_cell_measurement_temperature    173
_cell_measurement_theta_max      29.6
_cell_measurement_theta_min      1.4
_cell_volume                     2498.79(19)
_computing_publication_material  CIFGEN_IN_OpenMoleN_(_1997)
_computing_structure_refinement  LSFM_OpenMoleN_(_1997)
_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_diffrn_ambient_temperature      173
_diffrn_measurement_details
;
180 frames, 25 sec/frame, delta phi = 1.0 deg. Each frame measured 2 times.
Detector to crystal distance 25 mm.
;
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'π scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.077
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            22038
_diffrn_reflns_theta_max         29.55
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.951
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.48
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.161
_refine_ls_abs_structure_details ' ?'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.748
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     307
_refine_ls_number_reflns         3369
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.100
_refine_ls_R_factor_gt           0.039
_refine_ls_shift/esd_mean        0.001
_refine_ls_shift/su_max          0.004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4Fo²/(σ²(Fo²) + 0.0064 Fo⁴)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.093
_refine_ls_wR_factor_ref         0.055
_reflns_number_gt                3369
_reflns_number_total             6263
_reflns_threshold_expression     >3.0σ(I)
_cod_data_source_file            ic001339p_2.cif
_cod_data_source_block           st135
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '4Fo^2^/(\s^2^(Fo^2^) + 0.0064
Fo^4^)' was changed to 'calc'. New tag '_refine_ls_weighting_details'
was created. The value of the new tag was set to 'w =
4Fo^2^/(\s^2^(Fo^2^) + 0.0064 Fo^4^)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2498.8(4)
_cod_original_formula_sum        'C25 H24 N4 O Cl3 Fe'
_cod_database_code               4320153
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,1/2+y,1/2-z
-x,-y,-z
+x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_type_symbol
FE 0.66186(2) 0.41929(6) -0.05010(3) 0.0307(2) Uani ? ? Fe
CL1 0.74149(4) 0.4953(1) -0.11063(5) 0.0409(4) Uani ? ? Cl
CL2 0.57540(4) 0.5321(1) -0.16436(5) 0.0402(4) Uani ? ? Cl
CL3 0.67677(4) 0.6334(1) 0.05643(5) 0.0415(4) Uani ? ? Cl
N1 0.6555(1) 0.1791(3) -0.1224(2) 0.031(1) Uani ? ? N
C1 0.6067(2) 0.1305(4) -0.1980(2) 0.034(2) Uani ? ? C
C2 0.6086(2) -0.0166(5) -0.2448(2) 0.040(2) Uani ? ? C
C3 0.6619(2) -0.1186(5) -0.2122(3) 0.042(2) Uani ? ? C
C4 0.7119(2) -0.0728(5) -0.1336(3) 0.041(2) Uani ? ? C
C5 0.7071(2) 0.0774(4) -0.0901(2) 0.033(2) Uani ? ? C
C6 0.7603(2) 0.1376(4) -0.0046(2) 0.034(2) Uani ? ? C
N2 0.7328(1) 0.2415(4) 0.0541(2) 0.031(1) Uani ? ? N
C7 0.6977(2) 0.1275(5) 0.0989(3) 0.053(2) Uani ? ? C
C8 0.6282(1) 0.1700(4) 0.0798(2) 0.028(1) Uani ? ? C
C9 0.5934(1) 0.0834(4) 0.1260(2) 0.035(1) Uani ? ? C
C10 0.5280(2) 0.1147(5) 0.1040(2) 0.042(2) Uani ? ? C
C11 0.4995(1) 0.2318(4) 0.0359(2) 0.036(2) Uani ? ? C
C12 0.5369(1) 0.3145(4) -0.0068(2) 0.033(1) Uani ? ? C
N3 0.6009(1) 0.2852(3) 0.0139(2) 0.030(1) Uani ? ? N
C13 0.7852(2) 0.3389(4) 0.1240(2) 0.036(2) Uani ? ? C
C14 0.8440(2) 0.2383(4) 0.1771(2) 0.031(1) Uani ? ? C
N4 0.8918(1) 0.2388(3) 0.1401(2) 0.030(1) Uani ? ? N
C15 0.9456(2) 0.1482(4) 0.1807(2) 0.029(1) Uani ? ? C
C16 0.9529(2) 0.0556(4) 0.2619(2) 0.034(2) Uani ? ? C
C17 0.9043(2) 0.0578(5) 0.3007(2) 0.038(2) Uani ? ? C
C18 0.8487(2) 0.1504(5) 0.2586(2) 0.035(2) Uani ? ? C
C19 0.9956(1) 0.1523(4) 0.1349(2) 0.029(1) Uani ? ? C
C20 0.9825(2) 0.2320(4) 0.0484(2) 0.035(2) Uani ? ? C
C21 1.0276(2) 0.2397(5) 0.0033(2) 0.036(2) Uani ? ? C
C22 1.0875(2) 0.1658(4) 0.0428(2) 0.035(2) Uani ? ? C
C23 1.1016(2) 0.0847(5) 0.1287(2) 0.042(2) Uani ? ? C
C24 1.0561(2) 0.0785(5) 0.1732(2) 0.039(2) Uani ? ? C
O 1.1354(1) 0.1652(3) 0.0041(1) 0.046(1) Uani ? ? O
C25 1.1258(2) 0.2648(5) -0.0772(2) 0.051(2) Uani ? ? C
H1 0.5695 0.2001 -0.2200 0.0464 Uiso calc C1 H
H2 0.5735 -0.0470 -0.2988 0.0574 Uiso calc C2 H
H3 0.6643 -0.2202 -0.2438 0.0630 Uiso calc C3 H
H4 0.7488 -0.1427 -0.1096 0.0603 Uiso calc C4 H
H5 0.7902 0.2031 -0.0230 0.0472 Uiso calc C6 H
H6 0.7819 0.0432 0.0304 0.0472 Uiso calc C6 H
H7 0.7190 0.1315 0.1645 0.0716 Uiso calc C7 H
H8 0.7000 0.0164 0.0771 0.0716 Uiso calc C7 H
H9 0.6142 0.0030 0.1725 0.0442 Uiso calc C9 H
H10 0.5033 0.0568 0.1351 0.0519 Uiso calc C10 H
H11 0.4546 0.2548 0.0187 0.0475 Uiso calc C11 H
H12 0.5169 0.3962 -0.0530 0.0427 Uiso calc C12 H
H13 0.7676 0.3864 0.1677 0.0473 Uiso calc C13 H
H14 0.7986 0.4265 0.0920 0.0473 Uiso calc C13 H
H15 0.9911 -0.0082 0.2901 0.0473 Uiso calc C16 H
H16 0.9089 -0.0039 0.3560 0.0530 Uiso calc C17 H
H17 0.8148 0.1540 0.2845 0.0479 Uiso calc C18 H
H18 0.9413 0.2823 0.0200 0.0479 Uiso calc C20 H
H19 1.0175 0.2958 -0.0550 0.0491 Uiso calc C21 H
H20 1.1426 0.0335 0.1566 0.0573 Uiso calc C23 H
H21 1.0664 0.0224 0.2315 0.0532 Uiso calc C24 H
H22 1.1622 0.2542 -0.0975 0.0635 Uiso calc C25 H
H23 1.0881 0.2275 -0.1252 0.0635 Uiso calc C25 H
H24 1.1206 0.3793 -0.0632 0.0635 Uiso calc C25 H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1
H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1
N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1
O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1
Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1
Fe ? 0.301 0.845 International_Tables_Vol_IV_Table_2.3.1
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
CL1 FE CL2 98.07(4) . . . ?
CL1 FE CL3 97.92(4) . . . ?
CL1 FE N1 87.61(7) . . . ?
CL1 FE N2 90.41(7) . . . ?
CL1 FE N3 164.81(8) . . . ?
CL2 FE CL3 97.65(4) . . . ?
CL2 FE N1 93.58(8) . . . ?
CL2 FE N2 164.73(8) . . . ?
CL2 FE N3 93.11(8) . . . ?
CL3 FE N1 166.63(8) . . . ?
CL3 FE N2 93.71(8) . . . ?
CL3 FE N3 90.71(8) . . . ?
N1 FE N2 74.0(1) . . . ?
N1 FE N3 81.4(1) . . . ?
N2 FE N3 76.5(1) . . . ?
C1 N1 C5 118.4(3) . . . ?
N1 C1 C2 122.4(3) . . . ?
C1 C2 C3 118.9(4) . . . ?
C2 C3 C4 119.6(4) . . . ?
C3 C4 C5 118.6(4) . . . ?
N1 C5 C4 122.1(3) . . . ?
N1 C5 C6 116.1(3) . . . ?
C4 C5 C6 121.8(3) . . . ?
C5 C6 N2 110.1(3) . . . ?
C6 N2 C7 108.1(3) . . . ?
C6 N2 C13 110.3(2) . . . ?
C7 N2 C13 112.3(3) . . . ?
N2 C7 C8 114.9(3) . . . ?
C7 C8 C9 119.3(3) . . . ?
C7 C8 N3 118.3(3) . . . ?
C9 C8 N3 122.4(3) . . . ?
C8 C9 C10 119.4(3) . . . ?
C9 C10 C11 118.6(3) . . . ?
C10 C11 C12 119.1(3) . . . ?
C11 C12 N3 123.0(3) . . . ?
C8 N3 C12 117.5(3) . . . ?
N2 C13 C14 115.1(3) . . . ?
C13 C14 N4 115.0(3) . . . ?
C13 C14 C18 122.7(3) . . . ?
N4 C14 C18 122.3(3) . . . ?
C14 N4 C15 119.6(3) . . . ?
N4 C15 C16 120.7(3) . . . ?
N4 C15 C19 116.5(3) . . . ?
C16 C15 C19 122.8(3) . . . ?
C15 C16 C17 119.5(3) . . . ?
C16 C17 C18 119.8(3) . . . ?
C14 C18 C17 118.1(3) . . . ?
C15 C19 C20 119.9(3) . . . ?
C15 C19 C24 123.1(3) . . . ?
C20 C19 C24 117.0(3) . . . ?
C19 C20 C21 122.0(3) . . . ?
C20 C21 C22 120.0(3) . . . ?
C21 C22 C23 119.2(3) . . . ?
C21 C22 O 124.8(3) . . . ?
C23 C22 O 116.0(3) . . . ?
C22 C23 C24 120.2(3) . . . ?
C19 C24 C23 121.6(3) . . . ?
C22 O C25 117.3(3) . . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
FE CL1 2.3076(9) . . ?
FE CL2 2.286(1) . . ?
FE CL3 2.296(1) . . ?
FE N1 2.185(3) . . ?
FE N2 2.300(3) . . ?
FE N3 2.176(3) . . ?
N1 C1 1.341(4) . . ?
N1 C5 1.344(4) . . ?
C1 C2 1.377(5) . . ?
C2 C3 1.374(6) . . ?
C3 C4 1.375(6) . . ?
C4 C5 1.385(5) . . ?
C5 C6 1.507(5) . . ?
C6 N2 1.481(4) . . ?
N2 C7 1.493(4) . . ?
N2 C13 1.496(5) . . ?
C7 C8 1.492(5) . . ?
C8 C9 1.379(4) . . ?
C8 N3 1.343(4) . . ?
C9 C10 1.382(5) . . ?
C10 C11 1.378(5) . . ?
C11 C12 1.370(5) . . ?
C12 N3 1.352(4) . . ?
C13 C14 1.503(5) . . ?
C14 N4 1.344(4) . . ?
C14 C18 1.397(5) . . ?
N4 C15 1.345(4) . . ?
C15 C16 1.401(5) . . ?
C15 C19 1.480(5) . . ?
C16 C17 1.378(5) . . ?
C17 C18 1.384(5) . . ?
C19 C20 1.400(5) . . ?
C19 C24 1.390(5) . . ?
C20 C21 1.380(5) . . ?
C21 C22 1.380(5) . . ?
C22 C23 1.396(5) . . ?
C22 O 1.365(4) . . ?
C23 C24 1.378(5) . . ?
O C25 1.423(5) . . ?
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?
