#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:27:59 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179329 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/26/4322625.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_4322625
loop_
_publ_author_name
'Alain Diebold'
'Karl S. Hagen'
_publ_section_title
;
 Iron(II) Polyamine Chemistry: Variation of Spin State and Coordination
 Number in Solid State and Solution with Iron(II)
 Tris(2-pyridylmethyl)amine Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              215
_journal_page_last               223
_journal_paper_doi               10.1021/ic971105e
_journal_volume                  37
_journal_year                    1998
_chemical_formula_moiety         '[Fe(TPA)(CH3CN)2](SO3CF3)2(CH3CN)'
_chemical_formula_sum            'C26 H27 F6 Fe N7 O6 S2'
_chemical_formula_weight         767.52
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 92.09(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.418(2)
_cell_length_b                   16.192(4)
_cell_length_c                   15.855(2)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.49
_cell_measurement_theta_min      5.20
_cell_volume                     3185.9(10)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0599
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6846
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        5.22
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.692
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_description       fragment_of_plate
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          .40
_exptl_crystal_size_mid          .30
_exptl_crystal_size_min          .26
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.060
_refine_ls_goodness_of_fit_obs   1.070
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         5616
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_restrained_S_obs      1.070
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_obs          0.0441
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0516P)²+2.3878P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1189
_refine_ls_wR_factor_obs         0.1044
_reflns_number_observed          4345
_reflns_number_total             5616
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971105e_6.cif
_cod_data_source_block           C26H27F6FeN7O6S2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0516P)^2^+2.3878P] 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^)+(0.0516P)^2^+2.3878P] 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        3185.8(10)
_cod_database_code               4322625
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Fe Fe 0.22165(3) 0.08032(3) 0.34175(3) 0.01585(13) Uani 1 d . .
N1 N 0.3392(2) 0.0037(2) 0.3763(2) 0.0177(6) Uani 1 d . .
N2 N 0.2094(2) 0.0147(2) 0.2385(2) 0.0174(6) Uani 1 d . .
N3 N 0.1311(2) -0.0022(2) 0.3952(2) 0.0178(6) Uani 1 d . .
N4 N 0.3393(2) 0.1461(2) 0.2970(2) 0.0195(6) Uani 1 d . .
N5 N 0.1046(2) 0.1540(2) 0.3099(2) 0.0206(6) Uani 1 d . .
N6 N 0.2379(2) 0.1438(2) 0.4457(2) 0.0194(6) Uani 1 d . .
C1 C 0.1376(3) 0.0253(2) 0.1733(2) 0.0241(7) Uani 1 d . .
H1A H 0.0904(3) 0.0715(2) 0.1741(2) 0.029 Uiso 1 calc R .
C2 C 0.1303(3) -0.0281(2) 0.1059(2) 0.0336(9) Uani 1 d . .
H2A H 0.0787(3) -0.0191(2) 0.0612(2) 0.040 Uiso 1 calc R .
C3 C 0.1989(3) -0.0947(2) 0.1042(2) 0.0382(10) Uani 1 d . .
H3A H 0.1946(3) -0.1327(2) 0.0586(2) 0.046 Uiso 1 calc R .
C4 C 0.2737(3) -0.1058(2) 0.1694(2) 0.0313(8) Uani 1 d . .
H4A H 0.3226(3) -0.1509(2) 0.1688(2) 0.038 Uiso 1 calc R .
C5 C 0.2769(2) -0.0502(2) 0.2360(2) 0.0200(7) Uani 1 d . .
C6 C 0.3569(3) -0.0590(2) 0.3081(2) 0.0220(7) Uani 1 d . .
H6A H 0.4305(3) -0.0523(2) 0.2871(2) 0.026 Uiso 1 calc R .
H6B H 0.3513(3) -0.1152(2) 0.3322(2) 0.026 Uiso 1 calc R .
C7 C 0.0241(2) -0.0143(2) 0.3831(2) 0.0208(7) Uani 1 d . .
H7A H -0.0155(2) 0.0224(2) 0.3468(2) 0.025 Uiso 1 calc R .
C8 C -0.0299(3) -0.0776(2) 0.4212(2) 0.0243(7) Uani 1 d . .
H8A H -0.1052(3) -0.0844(2) 0.4110(2) 0.029 Uiso 1 calc R .
C9 C 0.0265(3) -0.1312(2) 0.4741(2) 0.0267(8) Uani 1 d . .
H9A H -0.0094(3) -0.1745(2) 0.5022(2) 0.032 Uiso 1 calc R .
C10 C 0.1374(3) -0.1202(2) 0.4855(2) 0.0252(7) Uani 1 d . .
H10A H 0.1786(3) -0.1570(2) 0.5204(2) 0.030 Uiso 1 calc R .
C11 C 0.1868(2) -0.0557(2) 0.4460(2) 0.0184(7) Uani 1 d . .
C12 C 0.3051(2) -0.0374(2) 0.4551(2) 0.0196(7) Uani 1 d . .
H12A H 0.3195(2) -0.0007(2) 0.5041(2) 0.024 Uiso 1 calc R .
H12B H 0.3461(2) -0.0893(2) 0.4643(2) 0.024 Uiso 1 calc R .
C13 C 0.3325(3) 0.2104(2) 0.2436(2) 0.0262(8) Uani 1 d . .
H13A H 0.2636(3) 0.2261(2) 0.2211(2) 0.031 Uiso 1 calc R .
C14 C 0.4214(3) 0.2543(2) 0.2204(2) 0.0349(9) Uani 1 d . .
H14A H 0.4136(3) 0.3008(2) 0.1842(2) 0.042 Uiso 1 calc R .
C15 C 0.5214(3) 0.2299(2) 0.2504(2) 0.0341(9) Uani 1 d . .
H15A H 0.5839(3) 0.2594(2) 0.2350(2) 0.041 Uiso 1 calc R .
C16 C 0.5305(3) 0.1625(2) 0.3030(2) 0.0275(8) Uani 1 d . .
H16A H 0.5993(3) 0.1435(2) 0.3227(2) 0.033 Uiso 1 calc R .
C17 C 0.4382(3) 0.1229(2) 0.3264(2) 0.0212(7) Uani 1 d . .
C18 C 0.4386(2) 0.0545(2) 0.3907(2) 0.0210(7) Uani 1 d . .
H18A H 0.5034(2) 0.0196(2) 0.3850(2) 0.025 Uiso 1 calc R .
H18B H 0.4402(2) 0.0780(2) 0.4483(2) 0.025 Uiso 1 calc R .
C19 C 0.0335(3) 0.1978(2) 0.2973(2) 0.0245(7) Uani 1 d . .
C20 C -0.0570(3) 0.2531(3) 0.2814(3) 0.0408(10) Uani 1 d . .
H20A H -0.0402(3) 0.2914(3) 0.2360(3) 0.049 Uiso 1 calc R .
H20B H -0.0709(3) 0.2844(3) 0.3328(3) 0.049 Uiso 1 calc R .
H20C H -0.1211(3) 0.2208(3) 0.2649(3) 0.049 Uiso 1 calc R .
C21 C 0.2447(2) 0.1857(2) 0.5034(2) 0.0197(7) Uani 1 d . .
C22 C 0.2498(3) 0.2396(2) 0.5776(2) 0.0289(8) Uani 1 d . .
H22A H 0.3127(3) 0.2759(2) 0.5749(2) 0.035 Uiso 0.50 calc PR .
H22B H 0.2559(3) 0.2058(2) 0.6288(2) 0.035 Uiso 0.50 calc PR .
H22C H 0.1842(3) 0.2731(2) 0.5787(2) 0.035 Uiso 0.50 calc PR .
S1 S 0.29460(7) 0.03888(6) 0.73656(6) 0.0294(2) Uani 1 d . .
O1 O 0.2422(2) 0.1168(2) 0.7471(2) 0.0497(8) Uani 1 d . .
O2 O 0.2746(3) 0.0008(2) 0.6565(2) 0.0529(8) Uani 1 d . .
O3 O 0.4046(2) 0.0357(2) 0.7667(2) 0.0482(8) Uani 1 d . .
C23 C 0.2279(3) -0.0292(2) 0.8091(2) 0.0319(8) Uani 1 d . .
F1 F 0.2617(2) -0.1066(2) 0.8010(2) 0.0671(8) Uani 1 d . .
F2 F 0.2466(2) -0.0095(2) 0.88783(15) 0.0661(8) Uani 1 d . .
F3 F 0.1222(2) -0.0288(2) 0.7953(2) 0.0713(9) Uani 1 d . .
S2 S 0.05597(8) 0.22977(6) 1.05165(6) 0.0306(2) Uani 1 d . .
O4 O 0.1396(3) 0.2525(2) 1.1123(2) 0.0495(8) Uani 1 d . .
O5 O 0.0013(2) 0.2988(2) 1.0126(2) 0.0453(7) Uani 1 d . .
O6 O -0.0122(2) 0.1636(2) 1.0775(2) 0.0443(7) Uani 1 d . .
C24 C 0.1308(3) 0.1841(2) 0.9672(2) 0.0377(9) Uani 1 d . .
F4 F 0.1970(2) 0.1253(2) 0.9968(2) 0.0677(8) Uani 1 d . .
F5 F 0.0670(2) 0.1517(2) 0.9082(2) 0.0667(8) Uani 1 d . .
F6 F 0.1915(2) 0.2397(2) 0.92934(15) 0.0501(6) Uani 1 d . .
N7 N -0.0248(3) -0.3367(2) 0.5179(3) 0.0568(10) Uani 1 d . .
C25 C 0.0182(4) -0.3799(3) 0.4741(3) 0.0425(10) Uani 1 d . .
C26 C 0.0712(4) -0.4365(3) 0.4172(3) 0.0524(12) Uani 1 d . .
H26A H 0.0990(4) -0.4842(3) 0.4492(3) 0.063 Uiso 0.50 calc PR .
H26B H 0.1311(4) -0.4080(3) 0.3910(3) 0.063 Uiso 0.50 calc PR .
H26C H 0.0193(4) -0.4553(3) 0.3733(3) 0.063 Uiso 0.50 calc PR .
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
N5 Fe N6 87.05(11) . . ?
N5 Fe N2 94.71(11) . . ?
N6 Fe N2 178.23(11) . . ?
N5 Fe N3 95.52(11) . . ?
N6 Fe N3 92.12(11) . . ?
N2 Fe N3 87.90(10) . . ?
N5 Fe N4 97.66(11) . . ?
N6 Fe N4 87.95(11) . . ?
N2 Fe N4 91.62(11) . . ?
N3 Fe N4 166.80(11) . . ?
N5 Fe N1 178.64(11) . . ?
N6 Fe N1 92.54(10) . . ?
N2 Fe N1 85.70(10) . . ?
N3 Fe N1 83.20(10) . . ?
N4 Fe N1 83.61(11) . . ?
C12 N1 C18 112.2(2) . . ?
C12 N1 C6 110.8(2) . . ?
C18 N1 C6 109.9(2) . . ?
C12 N1 Fe 106.4(2) . . ?
C18 N1 Fe 107.1(2) . . ?
C6 N1 Fe 110.4(2) . . ?
C5 N2 C1 118.1(3) . . ?
C5 N2 Fe 114.8(2) . . ?
C1 N2 Fe 127.0(2) . . ?
C7 N3 C11 118.0(3) . . ?
C7 N3 Fe 127.9(2) . . ?
C11 N3 Fe 113.9(2) . . ?
C13 N4 C17 118.0(3) . . ?
C13 N4 Fe 128.2(2) . . ?
C17 N4 Fe 113.8(2) . . ?
C19 N5 Fe 174.9(3) . . ?
C21 N6 Fe 175.1(3) . . ?
N2 C1 C2 122.5(3) . . ?
C1 C2 C3 119.0(3) . . ?
C2 C3 C4 119.3(3) . . ?
C3 C4 C5 119.2(3) . . ?
N2 C5 C4 121.9(3) . . ?
N2 C5 C6 116.7(3) . . ?
C4 C5 C6 121.4(3) . . ?
C5 C6 N1 112.1(3) . . ?
N3 C7 C8 122.5(3) . . ?
C7 C8 C9 119.4(3) . . ?
C8 C9 C10 118.4(3) . . ?
C11 C10 C9 119.6(3) . . ?
N3 C11 C10 122.1(3) . . ?
N3 C11 C12 114.0(3) . . ?
C10 C11 C12 124.0(3) . . ?
N1 C12 C11 108.4(2) . . ?
N4 C13 C14 122.5(3) . . ?
C15 C14 C13 119.0(3) . . ?
C14 C15 C16 119.4(3) . . ?
C15 C16 C17 118.9(3) . . ?
N4 C17 C16 122.2(3) . . ?
N4 C17 C18 114.8(3) . . ?
C16 C17 C18 122.9(3) . . ?
N1 C18 C17 108.7(2) . . ?
N5 C19 C20 179.7(4) . . ?
N6 C21 C22 178.2(3) . . ?
O2 S1 O3 114.5(2) . . ?
O2 S1 O1 114.8(2) . . ?
O3 S1 O1 115.2(2) . . ?
O2 S1 C23 103.5(2) . . ?
O3 S1 C23 102.6(2) . . ?
O1 S1 C23 104.0(2) . . ?
F2 C23 F3 107.4(3) . . ?
F2 C23 F1 106.2(3) . . ?
F3 C23 F1 107.6(3) . . ?
F2 C23 S1 112.9(3) . . ?
F3 C23 S1 111.4(3) . . ?
F1 C23 S1 111.0(2) . . ?
O6 S2 O5 115.4(2) . . ?
O6 S2 O4 114.8(2) . . ?
O5 S2 O4 114.1(2) . . ?
O6 S2 C24 103.2(2) . . ?
O5 S2 C24 104.3(2) . . ?
O4 S2 C24 102.8(2) . . ?
F5 C24 F6 106.6(3) . . ?
F5 C24 F4 108.4(3) . . ?
F6 C24 F4 106.8(3) . . ?
F5 C24 S2 112.1(3) . . ?
F6 C24 S2 111.7(3) . . ?
F4 C24 S2 111.0(3) . . ?
N7 C25 C26 178.7(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 N5 1.934(3) . ?
Fe N6 1.947(3) . ?
Fe N2 1.953(3) . ?
Fe N3 1.959(3) . ?
Fe N4 1.962(3) . ?
Fe N1 1.978(3) . ?
N1 C12 1.490(4) . ?
N1 C18 1.494(4) . ?
N1 C6 1.505(4) . ?
N2 C5 1.346(4) . ?
N2 C1 1.350(4) . ?
N3 C7 1.350(4) . ?
N3 C11 1.355(4) . ?
N4 C13 1.342(4) . ?
N4 C17 1.350(4) . ?
N5 C19 1.144(4) . ?
N6 C21 1.139(4) . ?
C1 C2 1.375(5) . ?
C2 C3 1.375(5) . ?
C3 C4 1.376(5) . ?
C4 C5 1.386(5) . ?
C5 C6 1.494(4) . ?
C7 C8 1.377(5) . ?
C8 C9 1.380(5) . ?
C9 C10 1.394(5) . ?
C10 C11 1.373(5) . ?
C11 C12 1.501(4) . ?
C13 C14 1.374(5) . ?
C14 C15 1.372(5) . ?
C15 C16 1.376(5) . ?
C16 C17 1.376(5) . ?
C17 C18 1.505(5) . ?
C19 C20 1.452(5) . ?
C21 C22 1.464(4) . ?
S1 O2 1.424(3) . ?
S1 O3 1.431(3) . ?
S1 O1 1.432(3) . ?
S1 C23 1.815(4) . ?
C23 F2 1.301(4) . ?
C23 F3 1.323(4) . ?
C23 F1 1.329(4) . ?
S2 O6 1.435(3) . ?
S2 O5 1.436(3) . ?
S2 O4 1.437(3) . ?
S2 C24 1.815(4) . ?
C24 F5 1.313(4) . ?
C24 F6 1.331(4) . ?
C24 F4 1.332(5) . ?
N7 C25 1.134(5) . ?
C25 C26 1.459(6) . ?
