#------------------------------------------------------------------------------
#$Date: 2016-03-23 04:07:30 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179277 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/97/4319735.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_4319735
loop_
_publ_author_name
'John M. Rowland'
'Marilyn Olmstead'
'Pradip K. Mascharak'
_publ_section_title
;
 Syntheses, Structures, and Reactivity of Low Spin Iron(III) Complexes
 Containing a Single Carboxamido Nitrogen in a [FeN5L] Chromophore
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2810
_journal_page_last               2817
_journal_paper_doi               10.1021/ic001127s
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C24 H26 Cl2 Fe N7 O5'
_chemical_formula_weight         619.27
_chemical_name_common            '[Fe(III)(PaPy3)Cl)]ClO4.2CH3CN'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 98.8510(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.4292(3)
_cell_length_b                   14.1990(5)
_cell_length_c                   11.3770(4)
_cell_measurement_reflns_used    7242
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.5
_cell_measurement_theta_min      2.3
_cell_volume                     1345.46(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 5.03, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12918
_diffrn_reflns_theta_full        31.49
_diffrn_reflns_theta_max         31.49
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        <0.1
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    0.808
_exptl_absorpt_correction_T_max  0.9777
_exptl_absorpt_correction_T_min  0.7994
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;SADABS, Sheldrick, G.M. An empirical absorption correction program based 
 on the method of Blessing, R. H., Acta Cryst. (1995). A51, 33-38.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             638
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.707
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.002(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         7385
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0328
_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)+(0.0431P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0746
_reflns_number_gt                6717
_reflns_number_total             7385
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic001127s_2.cif
_cod_data_source_block           djn145
_cod_original_cell_volume        1345.45(8)
_cod_database_code               4319735
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, 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
Fe Fe 0.80538(3) 0.161140(19) 0.20102(2) 0.01016(6) Uani 1 1 d . . .
Cl1 Cl 0.94052(5) 0.07320(3) 0.35223(4) 0.01369(9) Uani 1 1 d . . .
O1 O 0.6075(2) 0.38865(13) 0.03657(13) 0.0247(4) Uani 1 1 d . . .
N1 N 0.8213(2) 0.27956(13) 0.29401(14) 0.0132(3) Uani 1 1 d . . .
N2 N 0.6990(2) 0.23806(13) 0.08244(14) 0.0127(3) Uani 1 1 d . . .
N3 N 0.7636(2) 0.05668(13) 0.08401(14) 0.0122(3) Uani 1 1 d . . .
N4 N 1.00298(19) 0.17901(12) 0.12804(14) 0.0136(3) Uani 1 1 d . . .
N5 N 0.6018(2) 0.11505(12) 0.24903(13) 0.0118(3) Uani 1 1 d . . .
C1 C 0.8993(3) 0.29707(16) 0.40420(17) 0.0168(4) Uani 1 1 d . . .
H1 H 0.9584 0.2477 0.4471 0.020 Uiso 1 1 calc R . .
C2 C 0.8962(3) 0.38548(17) 0.45732(18) 0.0198(4) Uani 1 1 d . . .
H2 H 0.9537 0.3960 0.5348 0.024 Uiso 1 1 calc R . .
C3 C 0.8091(3) 0.45754(17) 0.39685(19) 0.0209(4) Uani 1 1 d . . .
H3 H 0.8035 0.5176 0.4327 0.025 Uiso 1 1 calc R . .
C4 C 0.7291(3) 0.44027(17) 0.28137(19) 0.0184(4) Uani 1 1 d . . .
H4 H 0.6689 0.4886 0.2372 0.022 Uiso 1 1 calc R . .
C5 C 0.7397(2) 0.35164(15) 0.23305(17) 0.0145(4) Uani 1 1 d . . .
C6 C 0.6724(3) 0.32865(16) 0.10623(18) 0.0152(4) Uani 1 1 d . . .
C7 C 0.6764(3) 0.19873(16) -0.03768(17) 0.0150(4) Uani 1 1 d . . .
H7A H 0.7723 0.2103 -0.0761 0.018 Uiso 1 1 calc R . .
H7B H 0.5818 0.2275 -0.0871 0.018 Uiso 1 1 calc R . .
C8 C 0.6507(3) 0.09374(16) -0.02303(17) 0.0153(4) Uani 1 1 d . . .
H8A H 0.6707 0.0602 -0.0956 0.018 Uiso 1 1 calc R . .
H8B H 0.5381 0.0819 -0.0122 0.018 Uiso 1 1 calc R . .
C9 C 0.9201(2) 0.02520(16) 0.05193(18) 0.0154(4) Uani 1 1 d . . .
H9A H 0.9029 -0.0044 -0.0278 0.018 Uiso 1 1 calc R . .
H9B H 0.9703 -0.0219 0.1103 0.018 Uiso 1 1 calc R . .
C10 C 1.0281(2) 0.10944(16) 0.05190(17) 0.0150(4) Uani 1 1 d . . .
C11 C 1.1482(3) 0.11563(18) -0.01926(19) 0.0211(5) Uani 1 1 d . . .
H11 H 1.1651 0.0657 -0.0715 0.025 Uiso 1 1 calc R . .
C12 C 1.2428(3) 0.19608(18) -0.0125(2) 0.0233(5) Uani 1 1 d . . .
H12 H 1.3229 0.2029 -0.0622 0.028 Uiso 1 1 calc R . .
C13 C 1.2190(3) 0.26635(18) 0.0677(2) 0.0215(5) Uani 1 1 d . . .
H13 H 1.2850 0.3209 0.0757 0.026 Uiso 1 1 calc R . .
C14 C 1.0967(2) 0.25577(16) 0.13620(18) 0.0164(4) Uani 1 1 d . . .
H14 H 1.0792 0.3043 0.1902 0.020 Uiso 1 1 calc R . .
C15 C 0.6819(3) -0.02003(15) 0.14185(18) 0.0136(4) Uani 1 1 d . . .
H15A H 0.7611 -0.0562 0.1974 0.016 Uiso 1 1 calc R . .
H15B H 0.6267 -0.0637 0.0811 0.016 Uiso 1 1 calc R . .
C16 C 0.5619(2) 0.02700(15) 0.20841(16) 0.0132(4) Uani 1 1 d . . .
C17 C 0.4204(2) -0.01625(16) 0.22705(17) 0.0151(4) Uani 1 1 d . . .
H17 H 0.3940 -0.0777 0.1971 0.018 Uiso 1 1 calc R . .
C18 C 0.3184(2) 0.03228(17) 0.29043(17) 0.0169(4) Uani 1 1 d . . .
H18 H 0.2209 0.0041 0.3046 0.020 Uiso 1 1 calc R . .
C19 C 0.3590(2) 0.12185(16) 0.33292(17) 0.0168(4) Uani 1 1 d . . .
H19 H 0.2901 0.1556 0.3765 0.020 Uiso 1 1 calc R . .
C20 C 0.5022(2) 0.16156(18) 0.31078(15) 0.0140(3) Uani 1 1 d . . .
H20 H 0.5305 0.2230 0.3399 0.017 Uiso 1 1 calc R . .
Cl2 Cl 0.39051(6) 0.22348(4) 0.64985(4) 0.01831(10) Uani 1 1 d . . .
O2 O 0.2360(2) 0.20716(17) 0.57834(16) 0.0388(5) Uani 1 1 d . . .
O3 O 0.5032(2) 0.25633(16) 0.57556(17) 0.0372(5) Uani 1 1 d . . .
O4 O 0.3760(2) 0.29167(14) 0.74096(15) 0.0291(4) Uani 1 1 d . . .
O5 O 0.4513(3) 0.13635(14) 0.70473(18) 0.0405(5) Uani 1 1 d . . .
N6 N 0.2296(3) 0.44691(18) 0.2546(2) 0.0384(6) Uani 1 1 d . . .
C21 C 0.3714(3) 0.4713(2) 0.4714(2) 0.0310(6) Uani 1 1 d . . .
H21A H 0.4188 0.4120 0.5038 0.047 Uiso 1 1 calc R . .
H21B H 0.2927 0.4933 0.5203 0.047 Uiso 1 1 calc R . .
H21C H 0.4560 0.5187 0.4719 0.047 Uiso 1 1 calc R . .
C22 C 0.2919(3) 0.45631(19) 0.3497(2) 0.0264(5) Uani 1 1 d . . .
N7 N 0.9385(3) 0.33764(19) 0.7791(2) 0.0374(6) Uani 1 1 d . . .
C23 C 0.8867(3) 0.1732(2) 0.6824(2) 0.0322(6) Uani 1 1 d . . .
H23A H 0.8892 0.1257 0.7452 0.048 Uiso 1 1 calc R . .
H23B H 0.9695 0.1586 0.6333 0.048 Uiso 1 1 calc R . .
H23C H 0.7810 0.1727 0.6326 0.048 Uiso 1 1 calc R . .
C24 C 0.9172(3) 0.26590(19) 0.7359(2) 0.0252(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 0.0000 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'
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 Fe N1 82.76(7) . . ?
N2 Fe N3 86.35(7) . . ?
N1 Fe N3 169.05(7) . . ?
N2 Fe N4 87.90(7) . . ?
N1 Fe N4 97.05(7) . . ?
N3 Fe N4 83.63(7) . . ?
N2 Fe N5 93.01(7) . . ?
N1 Fe N5 97.06(7) . . ?
N3 Fe N5 82.36(7) . . ?
N4 Fe N5 165.87(7) . . ?
N2 Fe Cl1 177.10(6) . . ?
N1 Fe Cl1 94.41(5) . . ?
N3 Fe Cl1 96.49(5) . . ?
N4 Fe Cl1 91.81(5) . . ?
N5 Fe Cl1 87.98(5) . . ?
C1 N1 C5 118.14(19) . . ?
C1 N1 Fe 129.60(15) . . ?
C5 N1 Fe 112.26(13) . . ?
C6 N2 C7 123.62(17) . . ?
C6 N2 Fe 119.67(14) . . ?
C7 N2 Fe 115.72(14) . . ?
C9 N3 C15 112.00(16) . . ?
C9 N3 C8 112.12(14) . . ?
C15 N3 C8 109.33(16) . . ?
C9 N3 Fe 108.38(12) . . ?
C15 N3 Fe 107.16(11) . . ?
C8 N3 Fe 107.63(13) . . ?
C14 N4 C10 119.32(18) . . ?
C14 N4 Fe 126.66(14) . . ?
C10 N4 Fe 113.47(14) . . ?
C20 N5 C16 119.19(18) . . ?
C20 N5 Fe 127.92(15) . . ?
C16 N5 Fe 112.84(13) . . ?
N1 C1 C2 122.0(2) . . ?
N1 C1 H1 119.0 . . ?
C2 C1 H1 119.0 . . ?
C3 C2 C1 119.7(2) . . ?
C3 C2 H2 120.1 . . ?
C1 C2 H2 120.1 . . ?
C2 C3 C4 118.7(2) . . ?
C2 C3 H3 120.7 . . ?
C4 C3 H3 120.7 . . ?
C5 C4 C3 118.7(2) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
N1 C5 C4 122.70(19) . . ?
N1 C5 C6 114.33(18) . . ?
C4 C5 C6 122.83(19) . . ?
O1 C6 N2 127.2(2) . . ?
O1 C6 C5 122.1(2) . . ?
N2 C6 C5 110.63(18) . . ?
N2 C7 C8 105.83(16) . . ?
N2 C7 H7A 110.6 . . ?
C8 C7 H7A 110.6 . . ?
N2 C7 H7B 110.6 . . ?
C8 C7 H7B 110.6 . . ?
H7A C7 H7B 108.7 . . ?
C7 C8 N3 110.21(17) . . ?
C7 C8 H8A 109.6 . . ?
N3 C8 H8A 109.6 . . ?
C7 C8 H8B 109.6 . . ?
N3 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
N3 C9 C10 108.68(17) . . ?
N3 C9 H9A 110.0 . . ?
C10 C9 H9A 110.0 . . ?
N3 C9 H9B 110.0 . . ?
C10 C9 H9B 110.0 . . ?
H9A C9 H9B 108.3 . . ?
N4 C10 C11 121.7(2) . . ?
N4 C10 C9 115.26(17) . . ?
C11 C10 C9 123.0(2) . . ?
C12 C11 C10 118.8(2) . . ?
C12 C11 H11 120.6 . . ?
C10 C11 H11 120.6 . . ?
C13 C12 C11 119.2(2) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C12 C13 C14 119.0(2) . . ?
C12 C13 H13 120.5 . . ?
C14 C13 H13 120.5 . . ?
N4 C14 C13 121.8(2) . . ?
N4 C14 H14 119.1 . . ?
C13 C14 H14 119.1 . . ?
N3 C15 C16 106.76(17) . . ?
N3 C15 H15A 110.4 . . ?
C16 C15 H15A 110.4 . . ?
N3 C15 H15B 110.4 . . ?
C16 C15 H15B 110.4 . . ?
H15A C15 H15B 108.6 . . ?
N5 C16 C17 121.98(18) . . ?
N5 C16 C15 115.38(17) . . ?
C17 C16 C15 122.64(19) . . ?
C16 C17 C18 118.4(2) . . ?
C16 C17 H17 120.8 . . ?
C18 C17 H17 120.8 . . ?
C19 C18 C17 119.86(19) . . ?
C19 C18 H18 120.1 . . ?
C17 C18 H18 120.1 . . ?
C18 C19 C20 118.97(19) . . ?
C18 C19 H19 120.5 . . ?
C20 C19 H19 120.5 . . ?
N5 C20 C19 121.6(2) . . ?
N5 C20 H20 119.2 . . ?
C19 C20 H20 119.2 . . ?
O4 Cl2 O3 109.96(12) . . ?
O4 Cl2 O5 109.22(12) . . ?
O3 Cl2 O5 107.98(13) . . ?
O4 Cl2 O2 110.18(12) . . ?
O3 Cl2 O2 109.86(12) . . ?
O5 Cl2 O2 109.60(13) . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N6 C22 C21 178.4(3) . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C24 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N7 C24 C23 178.5(3) . . ?
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 N2 1.8559(17) . ?
Fe N1 1.9801(18) . ?
Fe N3 1.9880(17) . ?
Fe N4 1.9885(16) . ?
Fe N5 1.9902(17) . ?
Fe Cl1 2.2833(5) . ?
O1 C6 1.233(3) . ?
N1 C1 1.346(3) . ?
N1 C5 1.362(3) . ?
N2 C6 1.340(3) . ?
N2 C7 1.461(2) . ?
N3 C9 1.491(2) . ?
N3 C15 1.494(3) . ?
N3 C8 1.520(3) . ?
N4 C14 1.341(3) . ?
N4 C10 1.352(3) . ?
N5 C20 1.347(2) . ?
N5 C16 1.357(3) . ?
C1 C2 1.395(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.379(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.403(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.382(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.503(3) . ?
C7 C8 1.519(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.503(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.393(3) . ?
C11 C12 1.389(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.387(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.393(3) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C16 1.509(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.386(3) . ?
C17 C18 1.387(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.385(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.390(3) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
Cl2 O4 1.4372(17) . ?
Cl2 O3 1.4426(19) . ?
Cl2 O5 1.444(2) . ?
Cl2 O2 1.4441(18) . ?
N6 C22 1.135(3) . ?
C21 C22 1.458(3) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
N7 C24 1.133(4) . ?
C23 C24 1.457(4) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
