#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/84/4318427.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_4318427
loop_
_publ_author_name
'Dohyun Moon'
'Myoung Soo Lah'
'Rico E. Del Sesto'
'Joel S. Miller'
_publ_section_title
;
 The Effect of Ligand Charge on the Coordination Geometry of an Fe(III)
 Ion: Five- and Six-Coordinate Fe(III) Complexes of
 Tris(2-benzimidazolylmethyl)amine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4708
_journal_page_last               4714
_journal_paper_doi               10.1021/ic011155q
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C29 H39 Fe N7 O5.5'
_chemical_formula_weight         629.52
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.328(1)
_cell_angle_beta                 109.334(1)
_cell_angle_gamma                118.218(1)
_cell_formula_units_Z            2
_cell_length_a                   12.1896(5)
_cell_length_b                   12.5237(5)
_cell_length_c                   12.9989(5)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.88
_cell_volume                     1523.99(11)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    ORTEP3
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      173(1)
_diffrn_measured_fraction_theta_full 0.908
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device_type  'SMART 1000 Diffractometer'
_diffrn_measurement_method       'Omega scan'
_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  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9846
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        <2.0
_exptl_absorpt_coefficient_mu    0.546
_exptl_absorpt_correction_T_max  0.9274
_exptl_absorpt_correction_T_min  0.7718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.627
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.0093(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         6893
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.138
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0913P)²+0.8526P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1341
_refine_ls_wR_factor_ref         0.1391
_reflns_number_gt                6174
_reflns_number_total             6893
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011155q_2.cif
_cod_data_source_block           complex3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_formula_sum        'C29 H39 Fe N7 O5.50'
_cod_database_code               4318427
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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 0.56371(3) 0.53683(2) 0.65500(2) 0.02075(11) Uani 1 1 d . . .
O1 O 0.5000 0.5000 0.5000 0.0242(4) Uani 1 2 d S . .
N1 N 0.64400(19) 0.58690(17) 0.86126(14) 0.0278(4) Uani 1 1 d . . .
N2 N 0.77351(18) 0.66552(16) 0.72765(14) 0.0261(3) Uani 1 1 d . . .
N3 N 0.99042(19) 0.79349(18) 0.88865(16) 0.0334(4) Uani 1 1 d . . .
N4 N 0.50177(18) 0.36414(16) 0.67031(14) 0.0256(3) Uani 1 1 d . . .
N5 N 0.4595(2) 0.23241(19) 0.77414(18) 0.0371(4) Uani 1 1 d . . .
N6 N 0.46421(18) 0.61714(16) 0.70011(15) 0.0261(3) Uani 1 1 d . . .
N7 N 0.4381(2) 0.72707(19) 0.83258(17) 0.0332(4) Uani 1 1 d . . .
H1N7 H 0.450(3) 0.766(3) 0.897(3) 0.040 Uiso 1 1 d . . .
C1 C 0.7912(2) 0.6249(2) 0.90990(18) 0.0327(4) Uani 1 1 d . . .
H1A H 0.7929 0.5473 0.9008 0.039 Uiso 1 1 calc R . .
H1B H 0.8432 0.6799 0.9933 0.039 Uiso 1 1 calc R . .
C2 C 0.8562(2) 0.6982(2) 0.84388(18) 0.0291(4) Uani 1 1 d . . .
C3 C 0.8675(2) 0.75073(19) 0.69430(18) 0.0267(4) Uani 1 1 d . . .
C4 C 0.8462(2) 0.7681(2) 0.5877(2) 0.0314(4) Uani 1 1 d . . .
H4 H 0.7587 0.7143 0.5207 0.038 Uiso 1 1 calc R . .
C5 C 0.9611(3) 0.8692(2) 0.5861(2) 0.0391(5) Uani 1 1 d . . .
H5 H 0.9501 0.8843 0.5168 0.047 Uiso 1 1 calc R . .
C6 C 1.0939(3) 0.9494(2) 0.6865(3) 0.0443(6) Uani 1 1 d . . .
H6 H 1.1684 1.0170 0.6824 0.053 Uiso 1 1 calc R . .
C7 C 1.1164(2) 0.9305(2) 0.7909(2) 0.0410(6) Uani 1 1 d . . .
H7 H 1.2051 0.9827 0.8566 0.049 Uiso 1 1 calc R . .
C8 C 1.0008(2) 0.8296(2) 0.7945(2) 0.0315(4) Uani 1 1 d . . .
C9 C 0.5497(3) 0.4664(2) 0.87351(19) 0.0329(5) Uani 1 1 d . . .
H9A H 0.4681 0.4638 0.8711 0.039 Uiso 1 1 calc R . .
H9B H 0.5990 0.4645 0.9483 0.039 Uiso 1 1 calc R . .
C10 C 0.5042(2) 0.3507(2) 0.77319(18) 0.0301(4) Uani 1 1 d . . .
C11 C 0.4219(3) 0.1571(2) 0.6609(2) 0.0352(5) Uani 1 1 d . . .
C12 C 0.3678(3) 0.0246(2) 0.6105(3) 0.0448(6) Uani 1 1 d . . .
H12 H 0.3493 -0.0293 0.6526 0.054 Uiso 1 1 calc R . .
C13 C 0.3430(3) -0.0237(2) 0.4970(2) 0.0436(6) Uani 1 1 d . . .
H13 H 0.3071 -0.1117 0.4617 0.052 Uiso 1 1 calc R . .
C14 C 0.3706(2) 0.0570(2) 0.4328(2) 0.0362(5) Uani 1 1 d . . .
H14 H 0.3530 0.0214 0.3560 0.043 Uiso 1 1 calc R . .
C15 C 0.4234(2) 0.1886(2) 0.48127(19) 0.0298(4) Uani 1 1 d . . .
H15 H 0.4414 0.2418 0.4385 0.036 Uiso 1 1 calc R . .
C16 C 0.4486(2) 0.23817(19) 0.59659(18) 0.0273(4) Uani 1 1 d . . .
C17 C 0.6352(3) 0.6963(2) 0.90853(18) 0.0325(4) Uani 1 1 d . . .
H17A H 0.7205 0.7796 0.9291 0.039 Uiso 1 1 calc R . .
H17B H 0.6238 0.6946 0.9788 0.039 Uiso 1 1 calc R . .
C18 C 0.5106(2) 0.6793(2) 0.81437(18) 0.0286(4) Uani 1 1 d . . .
C19 C 0.3350(2) 0.6948(2) 0.7226(2) 0.0314(4) Uani 1 1 d . . .
C20 C 0.2320(3) 0.7211(2) 0.6895(2) 0.0381(5) Uani 1 1 d . . .
H20 H 0.2217 0.7670 0.7453 0.046 Uiso 1 1 calc R . .
C21 C 0.1464(3) 0.6758(2) 0.5704(2) 0.0401(5) Uani 1 1 d . . .
H21 H 0.0768 0.6918 0.5451 0.048 Uiso 1 1 calc R . .
C22 C 0.1615(2) 0.6063(2) 0.4863(2) 0.0376(5) Uani 1 1 d . . .
H22 H 0.1017 0.5773 0.4065 0.045 Uiso 1 1 calc R . .
C23 C 0.2635(2) 0.5796(2) 0.5188(2) 0.0316(4) Uani 1 1 d . . .
H23 H 0.2725 0.5327 0.4627 0.038 Uiso 1 1 calc R . .
C24 C 0.3516(2) 0.62591(19) 0.63905(18) 0.0269(4) Uani 1 1 d . . .
O2 O 0.5126(3) 0.1496(2) 0.95119(17) 0.0497(5) Uani 1 1 d . . .
H1O2 H 0.491(4) 0.179(3) 0.895(3) 0.060 Uiso 1 1 d . . .
C25 C 0.5816(8) 0.0931(6) 0.9298(4) 0.124(2) Uani 1 1 d . . .
H25A H 0.6793 0.1607 0.9590 0.186 Uiso 1 1 calc R . .
H25B H 0.5394 0.0465 0.8464 0.186 Uiso 1 1 calc R . .
H25C H 0.5738 0.0334 0.9693 0.186 Uiso 1 1 calc R . .
O3 O 0.1562(2) 0.9035(2) 0.12590(17) 0.0566(6) Uani 1 1 d . . .
H1O3 H 0.126(4) 0.882(4) 0.054(3) 0.068 Uiso 1 1 d . . .
C26 C 0.1095(4) 0.9802(3) 0.1612(3) 0.0646(9) Uani 1 1 d . . .
H26A H 0.0765 0.9544 0.2163 0.097 Uiso 1 1 calc R . .
H26B H 0.0342 0.9669 0.0933 0.097 Uiso 1 1 calc R . .
H26C H 0.1862 1.0712 0.1981 0.097 Uiso 1 1 calc R . .
O4 O 0.2374(5) 0.4060(4) 0.8321(3) 0.1095(13) Uani 1 1 d . . .
H1O4 H 0.183(7) 0.418(7) 0.838(6) 0.131 Uiso 1 1 d . . .
C27 C 0.1611(4) 0.3179(4) 0.7146(3) 0.0802(11) Uani 1 1 d . . .
H27A H 0.1478 0.3625 0.6631 0.120 Uiso 1 1 calc R . .
H27B H 0.0710 0.2472 0.7008 0.120 Uiso 1 1 calc R . .
H27C H 0.2122 0.2835 0.6992 0.120 Uiso 1 1 calc R . .
O5 O 0.8779(4) 0.4936(4) 0.0976(6) 0.1000(17) Uani 0.705(3) 1 d P A 1
H1O5 H 0.9418 0.5540 0.0928 0.120 Uiso 0.705(3) 1 calc PR A 1
C28 C 0.9018(7) 0.3968(6) 0.1015(6) 0.0780(16) Uani 0.705(3) 1 d P A 1
H28A H 0.9458 0.3920 0.0534 0.117 Uiso 0.705(3) 1 calc PR A 1
H28B H 0.8137 0.3140 0.0723 0.117 Uiso 0.705(3) 1 calc PR A 1
H28C H 0.9626 0.4170 0.1815 0.117 Uiso 0.705(3) 1 calc PR A 1
O6 O 0.1260(7) 0.7202(5) 0.2096(6) 0.0676(16) Uani 0.638(16) 1 d P B 1
H1O6 H 0.1399 0.7848 0.1939 0.081 Uiso 0.638(16) 1 calc PR B 1
C29 C 0.2495(7) 0.7196(6) 0.2421(5) 0.0558(17) Uani 0.638(16) 1 d P B 1
H29A H 0.3314 0.8083 0.2800 0.084 Uiso 0.638(16) 1 calc PR B 1
H29B H 0.2464 0.6750 0.1727 0.084 Uiso 0.638(16) 1 calc PR B 1
H29C H 0.2537 0.6752 0.2955 0.084 Uiso 0.638(16) 1 calc PR B 1
O7 O 0.0480(16) 0.6705(16) 0.1768(10) 0.146(4) Uani 0.658(16) 1 d P C 2
H1O7 H 0.0749 0.7212 0.2419 0.175 Uiso 0.658(16) 1 calc PR C 2
C30 C 0.1359(19) 0.6241(17) 0.1866(13) 0.143(7) Uani 0.658(16) 1 d P C 2
H30A H 0.1632 0.6303 0.1253 0.214 Uiso 0.658(16) 1 calc PR C 2
H30B H 0.0853 0.5343 0.1788 0.214 Uiso 0.658(16) 1 calc PR C 2
H30C H 0.2185 0.6765 0.2622 0.214 Uiso 0.658(16) 1 calc PR C 2
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'
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
O1 Fe1 N4 104.93(5) . . ?
O1 Fe1 N2 105.11(5) . . ?
N4 Fe1 N2 114.94(7) . . ?
O1 Fe1 N6 103.86(5) . . ?
N4 Fe1 N6 113.23(7) . . ?
N2 Fe1 N6 113.34(7) . . ?
O1 Fe1 N1 178.50(4) . . ?
N4 Fe1 N1 75.52(6) . . ?
N2 Fe1 N1 75.87(7) . . ?
N6 Fe1 N1 74.67(6) . . ?
Fe1 O1 Fe1 180.0 . 2_666 ?
C17 N1 C9 112.22(17) . . ?
C17 N1 C1 112.10(17) . . ?
C9 N1 C1 112.93(17) . . ?
C17 N1 Fe1 107.18(12) . . ?
C9 N1 Fe1 106.56(12) . . ?
C1 N1 Fe1 105.28(12) . . ?
C2 N2 C3 103.77(17) . . ?
C2 N2 Fe1 119.42(14) . . ?
C3 N2 Fe1 136.30(13) . . ?
C2 N3 C8 104.03(17) . . ?
C10 N4 C16 103.67(16) . . ?
C10 N4 Fe1 120.51(14) . . ?
C16 N4 Fe1 135.81(13) . . ?
C10 N5 C11 104.06(18) . . ?
C18 N6 C24 105.35(17) . . ?
C18 N6 Fe1 118.50(14) . . ?
C24 N6 Fe1 136.15(14) . . ?
C18 N7 C19 107.25(18) . . ?
N1 C1 C2 107.81(16) . . ?
N3 C2 N2 115.9(2) . . ?
N3 C2 C1 124.98(19) . . ?
N2 C2 C1 119.10(19) . . ?
C4 C3 N2 131.39(19) . . ?
C4 C3 C8 121.5(2) . . ?
N2 C3 C8 107.11(18) . . ?
C5 C4 C3 117.0(2) . . ?
C4 C5 C6 121.6(2) . . ?
C7 C6 C5 121.6(2) . . ?
C6 C7 C8 117.5(2) . . ?
N3 C8 C7 130.0(2) . . ?
N3 C8 C3 109.17(19) . . ?
C7 C8 C3 120.7(2) . . ?
N1 C9 C10 107.98(16) . . ?
N5 C10 N4 116.00(19) . . ?
N5 C10 C9 124.70(18) . . ?
N4 C10 C9 119.23(18) . . ?
C12 C11 N5 130.2(2) . . ?
C12 C11 C16 120.9(2) . . ?
N5 C11 C16 108.85(19) . . ?
C13 C12 C11 117.9(2) . . ?
C12 C13 C14 121.3(2) . . ?
C15 C14 C13 121.5(2) . . ?
C14 C15 C16 117.5(2) . . ?
C15 C16 N4 131.70(18) . . ?
C15 C16 C11 120.9(2) . . ?
N4 C16 C11 107.42(18) . . ?
N1 C17 C18 107.19(17) . . ?
N6 C18 N7 113.03(19) . . ?
N6 C18 C17 121.62(18) . . ?
N7 C18 C17 125.29(19) . . ?
N7 C19 C20 131.7(2) . . ?
N7 C19 C24 106.28(19) . . ?
C20 C19 C24 122.1(2) . . ?
C21 C20 C19 116.8(2) . . ?
C20 C21 C22 121.6(2) . . ?
C23 C22 C21 121.7(2) . . ?
C22 C23 C24 117.2(2) . . ?
C23 C24 C19 120.6(2) . . ?
C23 C24 N6 131.32(19) . . ?
C19 C24 N6 108.09(18) . . ?
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 O1 1.7886(3) . ?
Fe1 N4 1.9955(16) . ?
Fe1 N2 2.0098(17) . ?
Fe1 N6 2.0639(17) . ?
Fe1 N1 2.3826(17) . ?
O1 Fe1 1.7886(3) 2_666 ?
N1 C17 1.475(3) . ?
N1 C9 1.478(3) . ?
N1 C1 1.479(3) . ?
N2 C2 1.366(3) . ?
N2 C3 1.400(3) . ?
N3 C2 1.318(3) . ?
N3 C8 1.395(3) . ?
N4 C10 1.367(2) . ?
N4 C16 1.400(3) . ?
N5 C10 1.318(3) . ?
N5 C11 1.400(3) . ?
N6 C18 1.336(3) . ?
N6 C24 1.405(3) . ?
N7 C18 1.337(3) . ?
N7 C19 1.389(3) . ?
C1 C2 1.492(3) . ?
C3 C4 1.396(3) . ?
C3 C8 1.406(3) . ?
C4 C5 1.384(3) . ?
C5 C6 1.404(4) . ?
C6 C7 1.375(4) . ?
C7 C8 1.402(3) . ?
C9 C10 1.502(3) . ?
C11 C12 1.395(3) . ?
C11 C16 1.406(3) . ?
C12 C13 1.370(4) . ?
C13 C14 1.403(4) . ?
C14 C15 1.385(3) . ?
C15 C16 1.393(3) . ?
C17 C18 1.493(3) . ?
C19 C20 1.397(3) . ?
C19 C24 1.404(3) . ?
C20 C21 1.376(4) . ?
C21 C22 1.402(4) . ?
C22 C23 1.387(3) . ?
C23 C24 1.392(3) . ?
O2 C25 1.392(4) . ?
O3 C26 1.416(3) . ?
O4 C27 1.400(5) . ?
O5 C28 1.379(6) . ?
O6 C29 1.427(7) . ?
O7 C30 1.423(11) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N7 H1N7 O2 0.83(3) 1.87(3) 2.692(3) 175(3) 2_667
O2 H1O2 N5 0.89(4) 1.81(4) 2.686(3) 172(3) .
O3 H1O3 N3 0.82(4) 1.93(4) 2.712(3) 158(4) 1_454
O4 H1O4 O5 0.77(6) 1.83(6) 2.558(6) 156(7) 2_666
O4 H1O4 O7 0.77(6) 2.41(7) 3.095(14) 149(7) 2_566
O5 H1O5 O6 0.82 1.99 2.635(7) 134.6 1_655
O6 H1O6 O3 0.82 1.81 2.620(6) 167.1 .
O7 H1O7 O4 0.82 3.05 3.095(14) 85.5 2_566
