#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:06:20 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179467 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/64/4336427.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_4336427
loop_
_publ_author_name
'Michaela Grau'
'Jason England'
'Rafael Torres Martin de Rosales'
'Henry S. Rzepa'
'Andrew J. P. White'
'George J. P. Britovsek'
_publ_section_title
;
 Coordination Equilibria Between Seven- and Five-coordinate Iron(II)
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11867
_journal_page_last               11874
_journal_paper_doi               10.1021/ic401416h
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C21 H25 Fe N5, 2(C F3 O3 S)'
_chemical_formula_sum            'C23 H25 F6 Fe N5 O6 S2'
_chemical_formula_weight         701.45
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 129.267(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.4112(9)
_cell_length_b                   10.5689(2)
_cell_length_c                   15.0745(6)
_cell_measurement_reflns_used    9408
_cell_measurement_temperature    173
_cell_measurement_theta_max      32.5625
_cell_measurement_theta_min      4.1608
_cell_volume                     2764.4(3)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 15.9863
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'OD Xcalibur 3'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) x-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_sigmaI/netI    0.0119
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13890
_diffrn_reflns_theta_full        31.50
_diffrn_reflns_theta_max         32.64
_diffrn_reflns_theta_min         4.23
_exptl_absorpt_coefficient_mu    0.787
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_correction_T_min  0.756
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) 
(compiled Jan 23 2012,18:06:46) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_description       tablets
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.4275
_exptl_crystal_size_mid          0.4100
_exptl_crystal_size_min          0.1819
_refine_diff_density_max         0.918
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         4741
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0526
_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)+(0.0990P)²+1.3233P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1409
_reflns_number_gt                4436
_reflns_number_total             4741
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401416h_si_001_3.cif
_cod_data_source_block           '[Fe(1)](OTf)2'
_cod_database_code               4336427
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Fe1 Fe 0.0000 0.60392(2) 0.2500 0.02112(10) Uani 1 2 d S
N1 N 0.0000 0.80100(14) 0.2500 0.0183(3) Uani 1 2 d S
C2 C 0.04990(7) 0.86385(12) 0.24496(10) 0.0193(2) Uani 1 1 d .
C3 C 0.05220(8) 0.99564(12) 0.24626(11) 0.0245(2) Uani 1 1 d .
H3A H 0.0884 1.0398 0.2446 0.029 Uiso 1 1 calc R
C4 C 0.0000 1.06048(17) 0.2500 0.0275(4) Uani 1 2 d S
H4A H 0.0000 1.1504 0.2500 0.033 Uiso 1 2 calc SR
C5 C 0.09884(8) 0.78244(13) 0.23087(12) 0.0239(2) Uani 1 1 d .
H5A H 0.0769 0.7835 0.1496 0.029 Uiso 1 1 calc R
H5B H 0.1516 0.8180 0.2774 0.029 Uiso 1 1 calc R
N6 N 0.10281(6) 0.65009(10) 0.26679(9) 0.01962(19) Uani 1 1 d .
C7 C 0.16452(7) 0.63507(13) 0.39219(11) 0.0230(2) Uani 1 1 d .
H7A H 0.1625 0.7063 0.4329 0.028 Uiso 1 1 calc R
H7B H 0.2155 0.6364 0.4107 0.028 Uiso 1 1 calc R
C8 C 0.15430(7) 0.51146(13) 0.43164(11) 0.0223(2) Uani 1 1 d .
N9 N 0.08075(6) 0.47807(10) 0.37953(9) 0.0216(2) Uani 1 1 d .
C10 C 0.06669(9) 0.37007(14) 0.41137(13) 0.0281(3) Uani 1 1 d .
H10A H 0.0148 0.3469 0.3745 0.034 Uiso 1 1 calc R
C11 C 0.12567(12) 0.29197(15) 0.49620(14) 0.0350(3) Uani 1 1 d .
H11A H 0.1144 0.2161 0.5168 0.042 Uiso 1 1 calc R
C12 C 0.20151(12) 0.32630(18) 0.55059(14) 0.0387(4) Uani 1 1 d .
H12A H 0.2428 0.2745 0.6093 0.046 Uiso 1 1 calc R
C13 C 0.21624(9) 0.43723(17) 0.51818(12) 0.0323(3) Uani 1 1 d .
H13A H 0.2677 0.4623 0.5543 0.039 Uiso 1 1 calc R
C14 C 0.11629(9) 0.56323(15) 0.20395(13) 0.0298(3) Uani 1 1 d .
H14A H 0.1627 0.5896 0.2154 0.045 Uiso 1 1 calc R
H14B H 0.0719 0.5657 0.1220 0.045 Uiso 1 1 calc R
H14C H 0.1233 0.4769 0.2328 0.045 Uiso 1 1 calc R
S20 S 0.132159(19) 0.75506(3) 0.61251(3) 0.02388(10) Uani 1 1 d .
O21 O 0.06893(8) 0.70824(14) 0.49991(12) 0.0421(3) Uani 1 1 d .
O22 O 0.11784(9) 0.75822(12) 0.69356(12) 0.0374(3) Uani 1 1 d .
O23 O 0.20724(8) 0.70990(13) 0.65724(13) 0.0406(3) Uani 1 1 d .
C20 C 0.13676(8) 0.92288(14) 0.58753(12) 0.0239(2) Uani 1 1 d .
F21 F 0.19085(6) 0.98314(11) 0.68461(10) 0.0412(2) Uani 1 1 d .
F22 F 0.15271(7) 0.93797(12) 0.51604(10) 0.0415(3) Uani 1 1 d .
F23 F 0.07036(6) 0.98239(10) 0.54048(10) 0.0374(2) 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 0.0000 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
N1 Fe1 N9 129.44(3) . 2
N1 Fe1 N9 129.44(3) . .
N9 Fe1 N9 101.12(6) 2 .
N1 Fe1 N6 77.23(3) . 2
N9 Fe1 N6 79.06(4) 2 2
N9 Fe1 N6 118.08(4) . 2
N1 Fe1 N6 77.23(3) . .
N9 Fe1 N6 118.08(4) 2 .
N9 Fe1 N6 79.06(4) . .
N6 Fe1 N6 154.45(6) 2 .
C2 N1 C2 120.75(15) . 2
C2 N1 Fe1 119.63(8) . .
C2 N1 Fe1 119.63(8) 2 .
N1 C2 C3 121.20(12) . .
N1 C2 C5 115.51(11) . .
C3 C2 C5 123.19(11) . .
C4 C3 C2 118.01(13) . .
C3 C4 C3 120.80(17) 2 .
N6 C5 C2 111.53(10) . .
C14 N6 C5 109.92(10) . .
C14 N6 C7 110.21(11) . .
C5 N6 C7 111.00(10) . .
C14 N6 Fe1 114.22(9) . .
C5 N6 Fe1 110.48(7) . .
C7 N6 Fe1 100.72(7) . .
N6 C7 C8 110.03(10) . .
N9 C8 C13 121.50(13) . .
N9 C8 C7 115.50(11) . .
C13 C8 C7 122.98(13) . .
C8 N9 C10 119.21(12) . .
C8 N9 Fe1 113.15(9) . .
C10 N9 Fe1 127.60(10) . .
N9 C10 C11 122.01(15) . .
C10 C11 C12 119.00(15) . .
C13 C12 C11 119.19(14) . .
C12 C13 C8 119.08(15) . .
O23 S20 O21 114.99(9) . .
O23 S20 O22 115.46(9) . .
O21 S20 O22 115.03(9) . .
O23 S20 C20 102.48(7) . .
O21 S20 C20 103.37(8) . .
O22 S20 C20 102.88(7) . .
F21 C20 F23 107.00(12) . .
F21 C20 F22 107.81(12) . .
F23 C20 F22 106.96(12) . .
F21 C20 S20 111.61(10) . .
F23 C20 S20 112.18(10) . .
F22 C20 S20 111.02(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N1 2.0829(15) .
Fe1 N9 2.0937(11) 2
Fe1 N9 2.0937(11) .
Fe1 N6 2.2073(10) 2
Fe1 N6 2.2073(10) .
N1 C2 1.3436(13) .
N1 C2 1.3436(13) 2
C2 C3 1.3935(17) .
C2 C5 1.5110(18) .
C3 C4 1.3874(17) .
C4 C3 1.3874(17) 2
C5 N6 1.4822(17) .
N6 C14 1.4811(17) .
N6 C7 1.4839(16) .
C7 C8 1.5116(19) .
C8 N9 1.3491(16) .
C8 C13 1.3971(19) .
N9 C10 1.3504(18) .
C10 C11 1.387(2) .
C11 C12 1.389(3) .
C12 C13 1.388(3) .
S20 O23 1.4413(13) .
S20 O21 1.4454(13) .
S20 O22 1.4467(12) .
S20 C20 1.8297(15) .
C20 F21 1.3309(18) .
C20 F23 1.3329(15) .
C20 F22 1.3425(16) .
