#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:40:45 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179857 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/53/7015390.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_7015390
loop_
_publ_author_name
'Coates, Cristina M.'
'Hagan, Kenton'
'Mitchell, Casey A.'
'Gorden, John D.'
'Goldsmith, Christian R.'
_publ_section_title
;
 Structural characterization of manganese and iron complexes with
 methylated derivatives of bis(2-pyridylmethyl)-1,2-ethanediamine
 reveals unanticipated conformational flexibility.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4048
_journal_page_last               4058
_journal_paper_doi               10.1039/c0dt01556c
_journal_volume                  40
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C18 H26 Cl2 Fe1 N4'
_chemical_formula_sum            'C18 H26 Cl2 Fe N4'
_chemical_formula_weight         425.18
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2010-03-17T21:44:16-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.6928(7)
_cell_length_b                   16.2440(8)
_cell_length_c                   18.0040(9)
_cell_measurement_reflns_used    4978
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.25
_cell_measurement_wavelength     0.71073
_cell_volume                     4004.6(3)
_computing_cell_refinement       'SMART, SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'ATOMS v6.1 (Shape Software, 2004)'
_computing_publication_material  'SHELXCIF-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.025
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            38744
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.028
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.41
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4978
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0625P)²+2.5089P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1136
_refine_ls_wR_factor_ref         0.118
_reflns_number_gt                4335
_reflns_number_total             4978
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt01556c.txt
_cod_data_source_block           sad2
_cod_database_code               7015390
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.97463(2) 0.218448(18) 0.598048(16) 0.02679(10) Uani 1 1 d . . .
Cl1 Cl 1.10801(4) 0.13470(3) 0.55681(3) 0.03321(13) Uani 1 1 d . . .
N1 N 1.01750(13) 0.31400(11) 0.50122(9) 0.0286(4) Uani 1 1 d . . .
C1 C 1.09715(19) 0.42080(15) 0.57623(14) 0.0395(5) Uani 1 1 d . . .
H1A H 1.076 0.3847 0.6153 0.059 Uiso 1 1 calc R . .
H1B H 1.0685 0.4742 0.5832 0.059 Uiso 1 1 calc R . .
H1C H 1.167 0.4255 0.5773 0.059 Uiso 1 1 calc R . .
C18 C 0.9739(2) 0.00028(17) 0.66161(19) 0.0605(9) Uani 1 1 d . . .
H18A H 1.0061 0.0344 0.6256 0.091 Uiso 1 1 calc R . .
H18B H 0.9436 -0.0455 0.637 0.091 Uiso 1 1 calc R . .
H18C H 1.021 -0.0196 0.6968 0.091 Uiso 1 1 calc R . .
Cl2 Cl 1.04713(5) 0.28255(4) 0.70459(3) 0.03868(15) Uani 1 1 d . . .
N2 N 0.88644(13) 0.18253(12) 0.49674(11) 0.0352(4) Uani 1 1 d . . .
C2 C 1.06593(16) 0.38673(13) 0.50323(13) 0.0329(4) Uani 1 1 d . . .
N3 N 0.82958(14) 0.28011(10) 0.62291(11) 0.0311(4) Uani 1 1 d . . .
C3 C 1.0886(2) 0.42974(16) 0.43881(15) 0.0456(6) Uani 1 1 d . . .
H3A H 1.1235 0.4787 0.4417 0.055 Uiso 1 1 calc R . .
N4 N 0.88564(14) 0.12959(11) 0.68239(11) 0.0349(4) Uani 1 1 d . . .
C4 C 1.0595(2) 0.40030(18) 0.37087(15) 0.0522(7) Uani 1 1 d . . .
H4A H 1.0729 0.4295 0.3276 0.063 Uiso 1 1 calc R . .
C5 C 1.0103(2) 0.32709(18) 0.36826(13) 0.0463(6) Uani 1 1 d . . .
H5A H 0.9895 0.3058 0.323 0.056 Uiso 1 1 calc R . .
C6 C 0.99190(18) 0.28475(14) 0.43387(12) 0.0345(5) Uani 1 1 d . . .
C7 C 0.94683(19) 0.20098(16) 0.43120(13) 0.0409(5) Uani 1 1 d . . .
H7A H 0.9067 0.1967 0.387 0.049 Uiso 1 1 calc R . .
H7B H 0.9983 0.1601 0.4274 0.049 Uiso 1 1 calc R . .
C8 C 0.8611(2) 0.09415(15) 0.49552(17) 0.0497(6) Uani 1 1 d . . .
H8A H 0.824 0.0822 0.4516 0.075 Uiso 1 1 calc R . .
H8B H 0.823 0.0809 0.5387 0.075 Uiso 1 1 calc R . .
H8C H 0.9199 0.0619 0.4955 0.075 Uiso 1 1 calc R . .
C9 C 0.79714(17) 0.23476(15) 0.49512(14) 0.0385(5) Uani 1 1 d . . .
H9A H 0.7487 0.21 0.4628 0.046 Uiso 1 1 calc R . .
H9B H 0.8132 0.2887 0.4755 0.046 Uiso 1 1 calc R . .
C10 C 0.75589(16) 0.24340(15) 0.57239(14) 0.0381(5) Uani 1 1 d . . .
H10A H 0.6983 0.2781 0.571 0.046 Uiso 1 1 calc R . .
H10B H 0.7367 0.1897 0.5909 0.046 Uiso 1 1 calc R . .
C11 C 0.83151(19) 0.37024(14) 0.61362(15) 0.0418(5) Uani 1 1 d . . .
H11A H 0.7682 0.3924 0.6248 0.063 Uiso 1 1 calc R . .
H11B H 0.8486 0.3834 0.5633 0.063 Uiso 1 1 calc R . .
H11C H 0.879 0.3935 0.6467 0.063 Uiso 1 1 calc R . .
C12 C 0.80446(18) 0.26207(14) 0.70068(14) 0.0380(5) Uani 1 1 d . . .
H12A H 0.7373 0.2783 0.7098 0.046 Uiso 1 1 calc R . .
H12B H 0.846 0.2944 0.7331 0.046 Uiso 1 1 calc R . .
C13 C 0.81630(16) 0.17216(14) 0.71924(12) 0.0334(5) Uani 1 1 d . . .
C14 C 0.75825(18) 0.13819(16) 0.77441(14) 0.0422(5) Uani 1 1 d . . .
H14A H 0.711 0.1697 0.7983 0.051 Uiso 1 1 calc R . .
C15 C 0.7721(2) 0.05695(18) 0.79308(14) 0.0469(6) Uani 1 1 d . . .
H15A H 0.7348 0.0327 0.8304 0.056 Uiso 1 1 calc R . .
C16 C 0.84164(19) 0.01200(15) 0.75593(14) 0.0428(5) Uani 1 1 d . . .
H16A H 0.8511 -0.0433 0.7673 0.051 Uiso 1 1 calc R . .
C17 C 0.89774(18) 0.04959(14) 0.70129(13) 0.0382(5) Uani 1 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 0 '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
N2 Fe1 N3 78.81(7) . . ?
N2 Fe1 Cl1 90.61(5) . . ?
N3 Fe1 Cl1 168.32(5) . . ?
N2 Fe1 Cl2 167.76(5) . . ?
N3 Fe1 Cl2 90.74(5) . . ?
Cl1 Fe1 Cl2 100.30(2) . . ?
N2 Fe1 N1 73.30(7) . . ?
N3 Fe1 N1 94.11(6) . . ?
Cl1 Fe1 N1 87.47(4) . . ?
Cl2 Fe1 N1 101.44(5) . . ?
N2 Fe1 N4 94.77(7) . . ?
N3 Fe1 N4 72.49(6) . . ?
Cl1 Fe1 N4 103.85(5) . . ?
Cl2 Fe1 N4 88.03(5) . . ?
N1 Fe1 N4 163.84(6) . . ?
C6 N1 C2 117.28(19) . . ?
C6 N1 Fe1 111.14(15) . . ?
C2 N1 Fe1 131.46(14) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C7 N2 C8 108.5(2) . . ?
C7 N2 C9 109.25(19) . . ?
C8 N2 C9 111.15(19) . . ?
C7 N2 Fe1 107.09(13) . . ?
C8 N2 Fe1 112.81(15) . . ?
C9 N2 Fe1 107.88(14) . . ?
N1 C2 C3 121.7(2) . . ?
N1 C2 C1 119.22(19) . . ?
C3 C2 C1 119.1(2) . . ?
C12 N3 C11 108.06(19) . . ?
C12 N3 C10 110.14(19) . . ?
C11 N3 C10 109.99(19) . . ?
C12 N3 Fe1 107.73(13) . . ?
C11 N3 Fe1 113.61(14) . . ?
C10 N3 Fe1 107.27(13) . . ?
C4 C3 C2 120.3(3) . . ?
C4 C3 H3A 119.9 . . ?
C2 C3 H3A 119.9 . . ?
C13 N4 C17 117.04(19) . . ?
C13 N4 Fe1 110.91(14) . . ?
C17 N4 Fe1 131.89(15) . . ?
C5 C4 C3 118.5(2) . . ?
C5 C4 H4A 120.8 . . ?
C3 C4 H4A 120.8 . . ?
C4 C5 C6 119.4(2) . . ?
C4 C5 H5A 120.3 . . ?
C6 C5 H5A 120.3 . . ?
N1 C6 C5 122.9(2) . . ?
N1 C6 C7 117.2(2) . . ?
C5 C6 C7 119.9(2) . . ?
N2 C7 C6 113.05(19) . . ?
N2 C7 H7A 109 . . ?
C6 C7 H7A 109 . . ?
N2 C7 H7B 109 . . ?
C6 C7 H7B 109 . . ?
H7A C7 H7B 107.8 . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 110.03(19) . . ?
N2 C9 H9A 109.7 . . ?
C10 C9 H9A 109.7 . . ?
N2 C9 H9B 109.7 . . ?
C10 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
N3 C10 C9 110.38(18) . . ?
N3 C10 H10A 109.6 . . ?
C9 C10 H10A 109.6 . . ?
N3 C10 H10B 109.6 . . ?
C9 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 C13 112.27(18) . . ?
N3 C12 H12A 109.2 . . ?
C13 C12 H12A 109.2 . . ?
N3 C12 H12B 109.2 . . ?
C13 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?
N4 C13 C14 123.5(2) . . ?
N4 C13 C12 117.60(19) . . ?
C14 C13 C12 118.9(2) . . ?
C15 C14 C13 118.6(2) . . ?
C15 C14 H14A 120.7 . . ?
C13 C14 H14A 120.7 . . ?
C16 C15 C14 119.1(2) . . ?
C16 C15 H15A 120.5 . . ?
C14 C15 H15A 120.5 . . ?
C15 C16 C17 119.6(2) . . ?
C15 C16 H16A 120.2 . . ?
C17 C16 H16A 120.2 . . ?
N4 C17 C16 122.1(2) . . ?
N4 C17 C18 118.6(2) . . ?
C16 C17 C18 119.2(2) . . ?
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 N2 2.2639(19) . ?
Fe1 N3 2.2689(18) . ?
Fe1 Cl1 2.3954(6) . ?
Fe1 Cl2 2.3978(6) . ?
Fe1 N1 2.4069(18) . ?
Fe1 N4 2.4236(19) . ?
N1 C6 1.349(3) . ?
N1 C2 1.355(3) . ?
C1 C2 1.489(3) . ?
C1 H1A 0.96 . ?
C1 H1B 0.96 . ?
C1 H1C 0.96 . ?
C18 C17 1.497(3) . ?
C18 H18A 0.96 . ?
C18 H18B 0.96 . ?
C18 H18C 0.96 . ?
N2 C7 1.472(3) . ?
N2 C8 1.477(3) . ?
N2 C9 1.489(3) . ?
C2 C3 1.389(3) . ?
N3 C12 1.471(3) . ?
N3 C11 1.474(3) . ?
N3 C10 1.484(3) . ?
C3 C4 1.372(4) . ?
C3 H3A 0.93 . ?
N4 C13 1.349(3) . ?
N4 C17 1.354(3) . ?
C4 C5 1.367(4) . ?
C4 H4A 0.93 . ?
C5 C6 1.390(3) . ?
C5 H5A 0.93 . ?
C6 C7 1.495(4) . ?
C7 H7A 0.97 . ?
C7 H7B 0.97 . ?
C8 H8A 0.96 . ?
C8 H8B 0.96 . ?
C8 H8C 0.96 . ?
C9 C10 1.508(4) . ?
C9 H9A 0.97 . ?
C9 H9B 0.97 . ?
C10 H10A 0.97 . ?
C10 H10B 0.97 . ?
C11 H11A 0.96 . ?
C11 H11B 0.96 . ?
C11 H11C 0.96 . ?
C12 C13 1.507(3) . ?
C12 H12A 0.97 . ?
C12 H12B 0.97 . ?
C13 C14 1.387(3) . ?
C14 C15 1.375(4) . ?
C14 H14A 0.93 . ?
C15 C16 1.374(4) . ?
C15 H15A 0.93 . ?
C16 C17 1.389(3) . ?
C16 H16A 0.93 . ?
