#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:24:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179749 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/45/7004511.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_7004511
loop_
_publ_author_name
'Benhamou, Laila'
'Lachkar, Mohammed'
'Mandon, Dominique'
'Welter, Richard'
_publ_section_title
;
 The preparation and full characterization of dichloroferrous complexes
 of mono-, bis- and tris-α-methyl substituted
 tris(2-pyridylmethyl)amine (TPA) ligands. Structural bases of
 stability of the complexes in solution
;
_journal_issue                   48
_journal_name_full               'Dalton Transactions'
_journal_page_first              6996
_journal_page_last               7003
_journal_paper_doi               10.1039/b808205g
_journal_year                    2008
_chemical_formula_moiety         'C19 H20 Cl2 Fe N4'
_chemical_formula_sum            'C19 H20 Cl2 Fe N4'
_chemical_formula_weight         431.14
_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                 119.29(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7940(3)
_cell_length_b                   27.979(3)
_cell_length_c                   8.8750(3)
_cell_measurement_reflns_used    4046
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      1.018
_cell_volume                     1904.5(10)
_computing_cell_refinement       'Denzo (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo (Nonius B.V., 1998)'
_computing_molecular_graphics    'PLATON 98 (Spek, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'π scans'
_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  0.0525
_diffrn_reflns_av_sigmaI/netI    0.1046
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7182
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         2.67
_exptl_absorpt_coefficient_mu    1.083
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.053
_refine_diff_density_min         -0.866
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         4519
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1429
_refine_ls_R_factor_gt           0.0735
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0566P)²+4.2057P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1394
_refine_ls_wR_factor_ref         0.1656
_reflns_number_gt                2707
_reflns_number_total             4519
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b808205g.txt
_cod_data_source_block           Me1TPAFeCl2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7004511
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.44867(8) 0.37517(2) 0.23210(8) 0.0329(2) Uani 1 1 d . . .
Cl1 Cl 0.65311(15) 0.31533(5) 0.22822(15) 0.0414(3) Uani 1 1 d . . .
Cl2 Cl 0.6292(5) 0.44247(13) 0.2968(12) 0.0576(17) Uani 0.87(2) 1 d P . .
Cl3 Cl 0.6539(14) 0.4338(6) 0.387(4) 0.035(5) Uani 0.13(2) 1 d P . .
N1 N 0.2251(5) 0.32211(13) 0.1403(5) 0.0339(9) Uani 1 1 d . . .
N2 N 0.4676(5) 0.34076(15) 0.4749(4) 0.0366(9) Uani 1 1 d . . .
N3 N 0.2307(5) 0.41830(14) 0.2217(5) 0.0341(9) Uani 1 1 d . . .
N4 N 0.2994(5) 0.38298(15) -0.0568(5) 0.0401(10) Uani 1 1 d . . .
C1 C 0.1851(6) 0.30734(19) -0.0349(6) 0.0460(13) Uani 1 1 d . . .
H1A H 0.0717 0.2904 -0.0918 0.055 Uiso 1 1 calc . . .
H1B H 0.2759 0.2849 -0.0267 0.055 Uiso 1 1 calc . . .
C2 C 0.1773(6) 0.3497(2) -0.1421(6) 0.0411(12) Uani 1 1 d . . .
C3 C 0.0578(7) 0.3531(2) -0.3151(7) 0.0566(16) Uani 1 1 d . . .
H3 H -0.0292 0.3292 -0.3695 0.068 Uiso 1 1 calc . . .
C4 C 0.0657(9) 0.3910(3) -0.4075(7) 0.071(2) Uani 1 1 d . . .
H4 H -0.0146 0.3938 -0.5275 0.085 Uiso 1 1 calc . . .
C5 C 0.1940(9) 0.4256(3) -0.3226(8) 0.0657(19) Uani 1 1 d . . .
H5 H 0.2024 0.4523 -0.3841 0.079 Uiso 1 1 calc . . .
C6 C 0.3089(7) 0.4205(2) -0.1477(7) 0.0491(14) Uani 1 1 d . . .
H6 H 0.3967 0.4440 -0.0901 0.059 Uiso 1 1 calc . . .
C7 C 0.0698(6) 0.34271(18) 0.1413(6) 0.0402(12) Uani 1 1 d . . .
H7A H 0.0547 0.3267 0.2324 0.048 Uiso 1 1 calc . . .
H7B H -0.0347 0.3357 0.0290 0.048 Uiso 1 1 calc . . .
C8 C 0.0793(5) 0.39575(17) 0.1715(5) 0.0320(10) Uani 1 1 d . . .
C9 C -0.0677(6) 0.41914(19) 0.1538(6) 0.0407(12) Uani 1 1 d . . .
H9 H -0.1733 0.4021 0.1187 0.049 Uiso 1 1 calc . . .
C10 C -0.0580(7) 0.4675(2) 0.1880(7) 0.0517(14) Uani 1 1 d . . .
H10 H -0.1572 0.4843 0.1758 0.062 Uiso 1 1 calc . . .
C11 C 0.0982(7) 0.49089(19) 0.2404(8) 0.0520(14) Uani 1 1 d . . .
H11 H 0.1086 0.5241 0.2659 0.062 Uiso 1 1 calc . . .
C12 C 0.2374(7) 0.46550(18) 0.2548(7) 0.0440(12) Uani 1 1 d . . .
H12 H 0.3441 0.4819 0.2899 0.053 Uiso 1 1 calc . . .
C13 C 0.2981(6) 0.28173(18) 0.2633(6) 0.0409(12) Uani 1 1 d . . .
H13A H 0.3886 0.2652 0.2471 0.049 Uiso 1 1 calc . . .
H13B H 0.2047 0.2584 0.2412 0.049 Uiso 1 1 calc . . .
C14 C 0.3752(6) 0.29986(18) 0.4428(6) 0.0386(11) Uani 1 1 d . . .
C15 C 0.3565(7) 0.2754(2) 0.5686(7) 0.0482(13) Uani 1 1 d . . .
H15 H 0.2874 0.2473 0.5406 0.058 Uiso 1 1 calc . . .
C16 C 0.4398(7) 0.2927(2) 0.7345(7) 0.0568(16) Uani 1 1 d . . .
H16 H 0.4320 0.2762 0.8239 0.068 Uiso 1 1 calc . . .
C17 C 0.5335(7) 0.3338(2) 0.7693(6) 0.0505(14) Uani 1 1 d . . .
H17 H 0.5914 0.3463 0.8835 0.061 Uiso 1 1 calc . . .
C18 C 0.5444(6) 0.3574(2) 0.6372(6) 0.0447(13) Uani 1 1 d . . .
C19 C 0.6327(9) 0.4023(3) 0.6719(9) 0.081(2) Uani 1 1 d . . .
H19A H 0.7281 0.4002 0.6449 0.121 Uiso 1 1 calc . . .
H19B H 0.6802 0.4104 0.7942 0.121 Uiso 1 1 calc . . .
H19C H 0.5505 0.4272 0.6003 0.121 Uiso 1 1 calc . . .
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'
Cl Cl 0.1484 0.1585 '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
N3 Fe1 N4 83.68(13) . . ?
N3 Fe1 N1 76.30(14) . . ?
N4 Fe1 N1 74.62(14) . . ?
N3 Fe1 N2 86.08(13) . . ?
N4 Fe1 N2 147.92(15) . . ?
N1 Fe1 N2 73.43(13) . . ?
N3 Fe1 Cl3 92.6(3) . . ?
N4 Fe1 Cl3 117.2(9) . . ?
N1 Fe1 Cl3 163.2(8) . . ?
N2 Fe1 Cl3 93.5(9) . . ?
N3 Fe1 Cl2 92.33(12) . . ?
N4 Fe1 Cl2 98.5(3) . . ?
N1 Fe1 Cl2 167.18(17) . . ?
N2 Fe1 Cl2 112.2(3) . . ?
Cl3 Fe1 Cl2 18.7(6) . . ?
N3 Fe1 Cl1 169.74(11) . . ?
N4 Fe1 Cl1 94.17(10) . . ?
N1 Fe1 Cl1 93.46(10) . . ?
N2 Fe1 Cl1 90.56(10) . . ?
Cl3 Fe1 Cl1 97.3(3) . . ?
Cl2 Fe1 Cl1 97.91(6) . . ?
C1 N1 C13 110.9(4) . . ?
C1 N1 C7 111.6(3) . . ?
C13 N1 C7 111.1(4) . . ?
C1 N1 Fe1 106.2(3) . . ?
C13 N1 Fe1 104.3(3) . . ?
C7 N1 Fe1 112.4(3) . . ?
C18 N2 C14 117.1(4) . . ?
C18 N2 Fe1 129.2(4) . . ?
C14 N2 Fe1 113.5(3) . . ?
C8 N3 C12 117.7(4) . . ?
C8 N3 Fe1 117.0(3) . . ?
C12 N3 Fe1 125.2(3) . . ?
C2 N4 C6 118.0(4) . . ?
C2 N4 Fe1 115.8(3) . . ?
C6 N4 Fe1 125.8(4) . . ?
N1 C1 C2 111.1(4) . . ?
N1 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
N1 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
N4 C2 C3 123.1(5) . . ?
N4 C2 C1 114.5(4) . . ?
C3 C2 C1 122.3(5) . . ?
C4 C3 C2 119.2(6) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C3 C4 C5 118.7(5) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
C6 C5 C4 119.3(6) . . ?
C6 C5 H5 120.4 . . ?
C4 C5 H5 120.4 . . ?
N4 C6 C5 121.6(6) . . ?
N4 C6 H6 119.2 . . ?
C5 C6 H6 119.2 . . ?
N1 C7 C8 114.4(4) . . ?
N1 C7 H7A 108.7 . . ?
C8 C7 H7A 108.7 . . ?
N1 C7 H7B 108.7 . . ?
C8 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
N3 C8 C9 122.4(5) . . ?
N3 C8 C7 119.0(4) . . ?
C9 C8 C7 118.6(4) . . ?
C10 C9 C8 118.9(4) . . ?
C10 C9 H9 120.5 . . ?
C8 C9 H9 120.5 . . ?
C9 C10 C11 118.9(5) . . ?
C9 C10 H10 120.5 . . ?
C11 C10 H10 120.5 . . ?
C12 C11 C10 118.9(5) . . ?
C12 C11 H11 120.6 . . ?
C10 C11 H11 120.6 . . ?
N3 C12 C11 123.2(5) . . ?
N3 C12 H12 118.4 . . ?
C11 C12 H12 118.4 . . ?
N1 C13 C14 109.7(4) . . ?
N1 C13 H13A 109.7 . . ?
C14 C13 H13A 109.7 . . ?
N1 C13 H13B 109.7 . . ?
C14 C13 H13B 109.7 . . ?
H13A C13 H13B 108.2 . . ?
N2 C14 C15 123.0(5) . . ?
N2 C14 C13 115.4(4) . . ?
C15 C14 C13 121.6(5) . . ?
C16 C15 C14 118.5(5) . . ?
C16 C15 H15 120.7 . . ?
C14 C15 H15 120.7 . . ?
C17 C16 C15 119.3(5) . . ?
C17 C16 H16 120.4 . . ?
C15 C16 H16 120.4 . . ?
C16 C17 C18 119.7(5) . . ?
C16 C17 H17 120.2 . . ?
C18 C17 H17 120.2 . . ?
N2 C18 C17 122.3(5) . . ?
N2 C18 C19 118.1(5) . . ?
C17 C18 C19 119.4(5) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 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 N3 2.228(4) . ?
Fe1 N4 2.248(4) . ?
Fe1 N1 2.273(4) . ?
Fe1 N2 2.290(4) . ?
Fe1 Cl3 2.326(11) . ?
Fe1 Cl2 2.346(2) . ?
Fe1 Cl1 2.4692(13) . ?
N1 C1 1.476(6) . ?
N1 C13 1.481(6) . ?
N1 C7 1.486(6) . ?
N2 C18 1.341(6) . ?
N2 C14 1.351(6) . ?
N3 C8 1.338(5) . ?
N3 C12 1.348(6) . ?
N4 C2 1.340(6) . ?
N4 C6 1.351(6) . ?
C1 C2 1.501(7) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.375(7) . ?
C3 C4 1.364(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.394(10) . ?
C4 H4 0.9500 . ?
C5 C6 1.384(8) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.503(7) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.387(6) . ?
C9 C10 1.379(7) . ?
C9 H9 0.9500 . ?
C10 C11 1.382(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.366(7) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.482(7) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.387(7) . ?
C15 C16 1.372(8) . ?
C15 H15 0.9500 . ?
C16 C17 1.358(8) . ?
C16 H16 0.9500 . ?
C17 C18 1.390(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.430(9) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
