#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:24:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179749 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/45/7004512.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_7004512
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         'C20 H22 Cl2 Fe N4'
_chemical_formula_sum            'C20 H22 Cl2 Fe N4'
_chemical_formula_weight         445.17
_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                 118.8660(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.88300(10)
_cell_length_b                   28.5770(5)
_cell_length_c                   8.9750(2)
_cell_measurement_reflns_used    5251
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     1995.22(6)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0661
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10121
_diffrn_reflns_theta_full        30.05
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    1.036
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5828
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0431
_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)+(0.0546P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1141
_reflns_number_gt                4169
_reflns_number_total             5828
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b808205g.txt
_cod_data_source_block           Me2TPAFeCl2
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7004512
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
Fe Fe 0.05073(3) 0.371767(10) 0.73155(4) 0.02278(10) Uani 1 1 d . . .
Cl1 Cl -0.14565(6) 0.312080(18) 0.73773(7) 0.03040(13) Uani 1 1 d . . .
Cl2 Cl -0.14254(6) 0.434279(18) 0.65128(7) 0.03028(13) Uani 1 1 d . . .
N1 N 0.2630(2) 0.31942(5) 0.8032(2) 0.0230(3) Uani 1 1 d . . .
N3 N 0.2605(2) 0.41432(6) 0.7388(2) 0.0246(4) Uani 1 1 d . . .
N2 N 0.0234(2) 0.34125(6) 0.4703(2) 0.0265(4) Uani 1 1 d . . .
N4 N 0.2189(2) 0.37515(5) 1.0318(2) 0.0233(4) Uani 1 1 d . . .
C1 C 0.4186(2) 0.34031(7) 0.8091(3) 0.0297(5) Uani 1 1 d . . .
H1A H 0.4410 0.3243 0.7239 0.036 Uiso 1 1 calc . . .
H1B H 0.5180 0.3342 0.9226 0.036 Uiso 1 1 calc . . .
C2 C 0.4079(2) 0.39222(7) 0.7757(2) 0.0229(4) Uani 1 1 d . . .
C3 C 0.5475(2) 0.41532(7) 0.7809(3) 0.0278(4) Uani 1 1 d . . .
H3 H 0.6500 0.3987 0.8072 0.033 Uiso 1 1 calc . . .
C4 C 0.5361(3) 0.46221(8) 0.7477(3) 0.0368(6) Uani 1 1 d . . .
H4 H 0.6304 0.4785 0.7500 0.044 Uiso 1 1 calc . . .
C5 C 0.3847(3) 0.48579(7) 0.7104(3) 0.0376(5) Uani 1 1 d . . .
H5 H 0.3739 0.5185 0.6880 0.045 Uiso 1 1 calc . . .
C6 C 0.2512(3) 0.46044(7) 0.7070(3) 0.0322(5) Uani 1 1 d . . .
H6 H 0.1474 0.4764 0.6809 0.039 Uiso 1 1 calc . . .
C7 C 0.1919(3) 0.28188(7) 0.6753(3) 0.0272(4) Uani 1 1 d . . .
H7A H 0.1031 0.2646 0.6895 0.033 Uiso 1 1 calc . . .
H7B H 0.2846 0.2596 0.6933 0.033 Uiso 1 1 calc . . .
C8 C 0.1139(2) 0.30125(7) 0.4978(3) 0.0265(4) Uani 1 1 d . . .
C9 C 0.1314(3) 0.27786(8) 0.3720(3) 0.0316(5) Uani 1 1 d . . .
H9 H 0.2004 0.2505 0.3977 0.038 Uiso 1 1 calc . . .
C10 C 0.0459(3) 0.29522(9) 0.2084(3) 0.0349(5) Uani 1 1 d . . .
H10 H 0.0526 0.2795 0.1184 0.042 Uiso 1 1 calc . . .
C11 C -0.0492(3) 0.33567(8) 0.1771(3) 0.0338(5) Uani 1 1 d . . .
H11 H -0.1097 0.3480 0.0650 0.041 Uiso 1 1 calc . . .
C12 C -0.0558(3) 0.35839(8) 0.3109(3) 0.0308(5) Uani 1 1 d . . .
C13 C -0.1528(3) 0.40352(9) 0.2807(3) 0.0453(6) Uani 1 1 d . . .
H13A H -0.2397 0.4002 0.3175 0.068 Uiso 1 1 calc . . .
H13B H -0.2093 0.4112 0.1592 0.068 Uiso 1 1 calc . . .
H13C H -0.0727 0.4286 0.3456 0.068 Uiso 1 1 calc . . .
C14 C 0.3007(3) 0.30022(7) 0.9702(3) 0.0282(4) Uani 1 1 d . . .
H14A H 0.4051 0.2805 1.0149 0.034 Uiso 1 1 calc . . .
H14B H 0.2039 0.2802 0.9566 0.034 Uiso 1 1 calc . . .
C15 C 0.3277(2) 0.33856(7) 1.0945(3) 0.0258(4) Uani 1 1 d . . .
C16 C 0.4524(2) 0.33481(8) 1.2642(3) 0.0329(5) Uani 1 1 d . . .
H16 H 0.5278 0.3087 1.3027 0.039 Uiso 1 1 calc . . .
C17 C 0.4649(3) 0.36968(8) 1.3758(3) 0.0362(5) Uani 1 1 d . . .
H17 H 0.5497 0.3682 1.4923 0.043 Uiso 1 1 calc . . .
C18 C 0.3524(3) 0.40664(8) 1.3150(3) 0.0339(5) Uani 1 1 d . . .
H18 H 0.3575 0.4307 1.3902 0.041 Uiso 1 1 calc . . .
C19 C 0.2309(2) 0.40883(7) 1.1433(3) 0.0262(4) Uani 1 1 d . . .
C20 C 0.1081(3) 0.44908(8) 1.0745(3) 0.0366(5) Uani 1 1 d . . .
H20A H 0.1327 0.4673 0.9962 0.055 Uiso 1 1 calc . . .
H20B H 0.1212 0.4691 1.1687 0.055 Uiso 1 1 calc . . .
H20C H -0.0099 0.4372 1.0136 0.055 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 Fe N1 77.14(6) . . ?
N3 Fe Cl2 94.15(4) . . ?
N1 Fe Cl2 171.23(4) . . ?
N3 Fe N4 83.33(6) . . ?
N1 Fe N4 73.75(6) . . ?
Cl2 Fe N4 106.58(4) . . ?
N3 Fe N2 85.09(6) . . ?
N1 Fe N2 73.29(6) . . ?
Cl2 Fe N2 105.28(4) . . ?
N4 Fe N2 146.73(6) . . ?
N3 Fe Cl1 169.33(4) . . ?
N1 Fe Cl1 92.19(4) . . ?
Cl2 Fe Cl1 96.52(2) . . ?
N4 Fe Cl1 93.85(4) . . ?
N2 Fe Cl1 91.82(4) . . ?
C7 N1 C14 108.85(15) . . ?
C7 N1 C1 111.25(16) . . ?
C14 N1 C1 111.29(16) . . ?
C7 N1 Fe 106.13(11) . . ?
C14 N1 Fe 106.63(11) . . ?
C1 N1 Fe 112.43(11) . . ?
C6 N3 C2 117.83(17) . . ?
C6 N3 Fe 124.88(13) . . ?
C2 N3 Fe 117.29(13) . . ?
C12 N2 C8 117.56(19) . . ?
C12 N2 Fe 131.33(14) . . ?
C8 N2 Fe 110.99(13) . . ?
C15 N4 C19 117.18(17) . . ?
C15 N4 Fe 112.00(13) . . ?
C19 N4 Fe 130.59(13) . . ?
N1 C1 C2 114.89(15) . . ?
N1 C1 H1A 108.5 . . ?
C2 C1 H1A 108.5 . . ?
N1 C1 H1B 108.5 . . ?
C2 C1 H1B 108.5 . . ?
H1A C1 H1B 107.5 . . ?
N3 C2 C3 122.29(18) . . ?
N3 C2 C1 118.18(17) . . ?
C3 C2 C1 119.52(17) . . ?
C4 C3 C2 119.31(18) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C3 C4 C5 119.21(19) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
C6 C5 C4 118.2(2) . . ?
C6 C5 H5 120.9 . . ?
C4 C5 H5 120.9 . . ?
N3 C6 C5 123.17(19) . . ?
N3 C6 H6 118.4 . . ?
C5 C6 H6 118.4 . . ?
N1 C7 C8 111.28(16) . . ?
N1 C7 H7A 109.4 . . ?
C8 C7 H7A 109.4 . . ?
N1 C7 H7B 109.4 . . ?
C8 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
N2 C8 C9 123.4(2) . . ?
N2 C8 C7 115.81(18) . . ?
C9 C8 C7 120.72(18) . . ?
C10 C9 C8 118.3(2) . . ?
C10 C9 H9 120.8 . . ?
C8 C9 H9 120.8 . . ?
C11 C10 C9 119.1(2) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
C10 C11 C12 119.6(2) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
N2 C12 C11 122.0(2) . . ?
N2 C12 C13 117.7(2) . . ?
C11 C12 C13 120.3(2) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N1 C14 C15 111.17(16) . . ?
N1 C14 H14A 109.4 . . ?
C15 C14 H14A 109.4 . . ?
N1 C14 H14B 109.4 . . ?
C15 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
N4 C15 C16 123.32(19) . . ?
N4 C15 C14 115.53(17) . . ?
C16 C15 C14 121.09(19) . . ?
C17 C16 C15 118.9(2) . . ?
C17 C16 H16 120.6 . . ?
C15 C16 H16 120.6 . . ?
C18 C17 C16 118.6(2) . . ?
C18 C17 H17 120.7 . . ?
C16 C17 H17 120.7 . . ?
C17 C18 C19 120.1(2) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
N4 C19 C18 121.90(19) . . ?
N4 C19 C20 117.29(18) . . ?
C18 C19 C20 120.81(19) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 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
Fe N3 2.1997(16) . ?
Fe N1 2.2441(15) . ?
Fe Cl2 2.3374(5) . ?
Fe N4 2.3695(17) . ?
Fe N2 2.4018(18) . ?
Fe Cl1 2.4594(5) . ?
N1 C7 1.472(2) . ?
N1 C14 1.475(3) . ?
N1 C1 1.483(3) . ?
N3 C6 1.343(3) . ?
N3 C2 1.343(2) . ?
N2 C12 1.346(3) . ?
N2 C8 1.350(2) . ?
N4 C15 1.349(2) . ?
N4 C19 1.355(2) . ?
C1 C2 1.507(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.386(3) . ?
C3 C4 1.366(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.393(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.378(3) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.503(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.384(3) . ?
C9 C10 1.380(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.378(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.391(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.501(3) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.498(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.389(3) . ?
C16 C17 1.379(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.373(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.391(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.498(3) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
