#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/14/7111486.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7111486
loop_
_publ_author_name
'Wong, Ella Lai-Ming'
'Fang, Guo-Su'
'Che, Chi-Ming'
'Zhu, Nianyong'
_publ_section_title
;
 Highly cytotoxic iron(ii) complexes with pentadentate pyridyl ligands as
 a new class of anti-tumor agents
;
_journal_issue                   36
_journal_name_full               'Chemical Communications'
_journal_page_first              4578
_journal_page_last               4580
_journal_paper_doi               10.1039/b507687k
_journal_year                    2005
_chemical_formula_moiety         'C32 H27.50 Cl2 Fe N8.50 O8'
_chemical_formula_sum            'C32 H27.5 Cl2 Fe N8.5 O8'
_chemical_formula_weight         785.88
_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                94.77(3)
_cell_angle_beta                 113.14(3)
_cell_angle_gamma                104.39(3)
_cell_formula_units_Z            2
_cell_length_a                   11.732(2)
_cell_length_b                   12.453(3)
_cell_length_c                   13.997(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     1783.5(9)
_computing_cell_refinement       Scalepack
_computing_data_collection       MarControl
_computing_data_reduction        Denzo
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      301(2)
_diffrn_measured_fraction_theta_full 0.550
_diffrn_measured_fraction_theta_max 0.550
_diffrn_measurement_device_type  'Marresearch Imaging Plate mar300'
_diffrn_measurement_method       Oscillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_sigmaI/netI    0.1367
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4652
_diffrn_reflns_theta_full        23.85
_diffrn_reflns_theta_max         23.85
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         3030
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.1518
_refine_ls_R_factor_gt           0.0941
_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)+(0.1848P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2494
_refine_ls_wR_factor_ref         0.2811
_reflns_number_gt                1514
_reflns_number_total             3030
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b507687ksup1.cif
_cod_data_source_block           Complex_1a
_cod_original_cell_volume        1783.5(7)
_cod_original_formula_sum        'C32 H27.50 Cl2 Fe N8.50 O8'
_cod_database_code               7111486
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 0.75393(16) 0.24645(15) 0.24676(12) 0.0737(8) Uani 1 1 d . . .
N1 N 0.5309(10) 0.1642(8) 0.1993(10) 0.075(3) Uani 1 1 d . . .
N2 N 0.6432(12) 0.1791(8) 0.0704(8) 0.071(3) Uani 1 1 d . . .
N3 N 0.8912(11) 0.2345(8) 0.1729(12) 0.081(3) Uani 1 1 d . . .
N4 N 0.9630(12) 0.3034(9) 0.3727(11) 0.089(3) Uani 1 1 d . . .
N5 N 0.7608(14) 0.3405(9) 0.3971(9) 0.087(3) Uani 1 1 d . . .
N6 N 0.7404(11) 0.4040(10) 0.1924(9) 0.088(4) Uani 1 1 d . . .
N7 N 0.7632(10) 0.0934(10) 0.3111(9) 0.093(4) Uani 1 1 d . . .
C1 C 0.4800(17) 0.1379(13) 0.2688(12) 0.096(4) Uani 1 1 d . . .
H1 H 0.5364 0.1521 0.3405 0.115 Uiso 1 1 calc R . .
C2 C 0.350(2) 0.0915(13) 0.2389(17) 0.106(5) Uani 1 1 d . . .
H2 H 0.3182 0.0741 0.2887 0.127 Uiso 1 1 calc R . .
C3 C 0.2687(16) 0.0712(13) 0.134(2) 0.116(6) Uani 1 1 d . . .
H3 H 0.1793 0.0429 0.1120 0.139 Uiso 1 1 calc R . .
C4 C 0.3161(16) 0.0919(13) 0.0596(13) 0.099(5) Uani 1 1 d . . .
H4 H 0.2607 0.0748 -0.0125 0.119 Uiso 1 1 calc R . .
C5 C 0.4504(15) 0.1394(11) 0.0961(13) 0.082(4) Uani 1 1 d . . .
C6 C 0.5173(16) 0.1586(10) 0.0249(12) 0.079(4) Uani 1 1 d . . .
C7 C 0.4439(16) 0.1557(13) -0.0834(14) 0.106(5) Uani 1 1 d . . .
H7 H 0.3546 0.1445 -0.1120 0.128 Uiso 1 1 calc R . .
C8 C 0.510(2) 0.1701(16) -0.1422(14) 0.131(7) Uani 1 1 d . . .
H8 H 0.4668 0.1678 -0.2144 0.158 Uiso 1 1 calc R . .
C9 C 0.641(2) 0.1879(14) -0.0980(16) 0.123(6) Uani 1 1 d . . .
H9 H 0.6859 0.1959 -0.1401 0.147 Uiso 1 1 calc R . .
C10 C 0.7072(17) 0.1943(11) 0.0099(14) 0.087(4) Uani 1 1 d . . .
C11 C 0.8461(19) 0.2137(11) 0.0659(15) 0.096(4) Uani 1 1 d . . .
C12 C 0.934(2) 0.2151(13) 0.0209(17) 0.129(6) Uani 1 1 d . . .
H12 H 0.9062 0.1996 -0.0522 0.155 Uiso 1 1 calc R . .
C13 C 1.067(3) 0.2415(18) 0.093(3) 0.156(9) Uani 1 1 d . . .
H13 H 1.1279 0.2456 0.0656 0.187 Uiso 1 1 calc R . .
C14 C 1.109(2) 0.2605(17) 0.197(2) 0.131(7) Uani 1 1 d . . .
H14 H 1.1967 0.2756 0.2424 0.158 Uiso 1 1 calc R . .
C15 C 1.0161(18) 0.2567(12) 0.2341(18) 0.095(4) Uani 1 1 d . . .
C16 C 1.0538(14) 0.2838(12) 0.3466(18) 0.096(5) Uani 1 1 d . . .
C17 C 1.170(2) 0.2889(16) 0.422(2) 0.144(8) Uani 1 1 d . . .
H17 H 1.2344 0.2744 0.4047 0.172 Uiso 1 1 calc R . .
C18 C 1.192(2) 0.3175(18) 0.531(3) 0.173(14) Uani 1 1 d . . .
H18 H 1.2714 0.3194 0.5842 0.208 Uiso 1 1 calc R . .
C19 C 1.102(2) 0.3414(16) 0.5568(15) 0.134(7) Uani 1 1 d . . .
H19 H 1.1173 0.3628 0.6270 0.161 Uiso 1 1 calc R . .
C20 C 0.9814(18) 0.3322(12) 0.4704(16) 0.097(5) Uani 1 1 d . . .
C21 C 0.875(2) 0.3544(12) 0.4837(12) 0.096(5) Uani 1 1 d . . .
C22 C 0.887(2) 0.3995(17) 0.5834(19) 0.144(8) Uani 1 1 d . . .
H22 H 0.9612 0.4081 0.6449 0.173 Uiso 1 1 calc R . .
C23 C 0.785(3) 0.4302(15) 0.5871(15) 0.137(8) Uani 1 1 d . . .
H23 H 0.7937 0.4603 0.6536 0.165 Uiso 1 1 calc R . .
C24 C 0.672(2) 0.4211(14) 0.5028(18) 0.117(5) Uani 1 1 d . . .
H24 H 0.6042 0.4435 0.5075 0.141 Uiso 1 1 calc R . .
C25 C 0.6704(17) 0.3727(11) 0.4055(12) 0.095(4) Uani 1 1 d . . .
H25 H 0.5966 0.3641 0.3434 0.114 Uiso 1 1 calc R . .
C26 C 0.7195(13) 0.4773(17) 0.1527(10) 0.093(5) Uani 1 1 d . . .
C27 C 0.6954(16) 0.5792(13) 0.1039(11) 0.117(5) Uani 1 1 d . . .
C28 C 0.7836(13) 0.0275(14) 0.3601(12) 0.087(4) Uani 1 1 d . . .
C29 C 0.8137(18) -0.0630(15) 0.4259(12) 0.135(6) Uani 1 1 d . . .
Cl1 Cl 0.9893(4) -0.1079(4) 0.2363(3) 0.1252(15) Uiso 1 1 d D . .
Cl2 Cl 0.4128(4) 0.5173(5) 0.2269(4) 0.152(2) Uani 1 1 d D . .
O1 O 0.8599(18) -0.1494(17) 0.2311(16) 0.137(7) Uiso 0.50 1 d PD A 1
O2 O 0.985(3) -0.038(2) 0.163(2) 0.216(12) Uiso 0.50 1 d PD A 1
O3 O 1.026(2) -0.2032(18) 0.2136(19) 0.182(10) Uiso 0.50 1 d PD A 1
O4 O 1.077(2) -0.049(3) 0.3411(18) 0.28(2) Uiso 0.50 1 d PD A 1
O1' O 0.993(3) -0.177(2) 0.309(2) 0.228(13) Uiso 0.50 1 d PD A 2
O2' O 1.063(2) 0.003(2) 0.294(2) 0.176(10) Uiso 0.50 1 d PD A 2
O3' O 1.052(3) -0.139(3) 0.179(2) 0.283(19) Uiso 0.50 1 d PD A 2
O4' O 0.867(3) -0.110(3) 0.173(2) 0.33(3) Uiso 0.50 1 d PD A 2
O5 O 0.4123(17) 0.4253(14) 0.1569(13) 0.297(10) Uiso 1 1 d D . .
O6 O 0.3051(14) 0.5460(14) 0.1766(11) 0.239(7) Uiso 1 1 d D . .
O7 O 0.4103(13) 0.4684(12) 0.3126(10) 0.207(6) Uiso 1 1 d D . .
O8 O 0.5247(13) 0.5988(12) 0.2529(11) 0.227(7) Uiso 1 1 d D . .
N8 N 0.005(4) 0.534(4) 0.141(3) 0.195(16) Uiso 0.50 1 d P . .
C30 C -0.014(4) 0.519(3) 0.034(3) 0.093(13) Uiso 0.50 1 d P . .
C31 C -0.004(5) 0.490(4) -0.073(4) 0.13(2) Uiso 0.50 1 d P . .
N9 N 0.445(3) 0.153(3) 0.517(2) 0.307(13) Uiso 1 1 d . . .
C32 C 0.544(3) 0.143(2) 0.576(2) 0.195(9) Uiso 1 1 d . . .
C33 C 0.678(2) 0.164(2) 0.6292(17) 0.190(8) Uiso 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Fe Fe 0.3463 0.8444 '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'
C C 0.0033 0.0016 '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'
O O 0.0106 0.0060 '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'
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
N6 Fe1 N7 175.4(4) . .
N6 Fe1 N2 80.1(4) . .
N7 Fe1 N2 103.2(4) . .
N6 Fe1 N3 89.7(4) . .
N7 Fe1 N3 94.5(4) . .
N2 Fe1 N3 69.2(5) . .
N6 Fe1 N4 100.6(4) . .
N7 Fe1 N4 79.2(4) . .
N2 Fe1 N4 138.7(5) . .
N3 Fe1 N4 69.5(6) . .
N6 Fe1 N5 83.3(4) . .
N7 Fe1 N5 92.3(4) . .
N2 Fe1 N5 147.6(5) . .
N3 Fe1 N5 138.5(5) . .
N4 Fe1 N5 71.7(5) . .
N6 Fe1 N1 97.1(4) . .
N7 Fe1 N1 81.2(4) . .
N2 Fe1 N1 69.1(5) . .
N3 Fe1 N1 135.8(4) . .
N4 Fe1 N1 149.2(5) . .
N5 Fe1 N1 85.7(5) . .
C5 N1 C1 118.3(12) . .
C5 N1 Fe1 117.2(10) . .
C1 N1 Fe1 124.5(10) . .
C6 N2 C10 118.0(12) . .
C6 N2 Fe1 119.8(10) . .
C10 N2 Fe1 118.9(10) . .
C15 N3 C11 120.4(15) . .
C15 N3 Fe1 119.6(13) . .
C11 N3 Fe1 119.7(10) . .
C20 N4 C16 123.2(16) . .
C20 N4 Fe1 116.9(12) . .
C16 N4 Fe1 118.4(11) . .
C25 N5 C21 121.3(14) . .
C25 N5 Fe1 126.7(11) . .
C21 N5 Fe1 111.9(12) . .
C26 N6 Fe1 171.0(13) . .
C28 N7 Fe1 167.9(12) . .
N1 C1 C2 123.0(14) . .
C1 C2 C3 117.9(16) . .
C2 C3 C4 121.2(16) . .
C3 C4 C5 117.5(15) . .
N1 C5 C4 121.8(15) . .
N1 C5 C6 114.3(13) . .
C4 C5 C6 123.7(15) . .
N2 C6 C7 124.8(14) . .
N2 C6 C5 115.6(13) . .
C7 C6 C5 119.7(16) . .
C8 C7 C6 115.9(16) . .
C7 C8 C9 120.7(17) . .
C8 C9 C10 120.1(17) . .
N2 C10 C9 120.5(15) . .
N2 C10 C11 114.6(15) . .
C9 C10 C11 124.9(18) . .
N3 C11 C12 119.4(17) . .
N3 C11 C10 113.7(15) . .
C12 C11 C10 126.9(19) . .
C11 C12 C13 116.2(19) . .
C14 C13 C12 124(2) . .
C13 C14 C15 116(2) . .
N3 C15 C14 124.2(19) . .
N3 C15 C16 115.6(16) . .
C14 C15 C16 120.1(19) . .
N4 C16 C17 120(2) . .
N4 C16 C15 114.9(14) . .
C17 C16 C15 125(2) . .
C16 C17 C18 118(2) . .
C19 C18 C17 122(2) . .
C18 C19 C20 116(2) . .
N4 C20 C21 115.7(16) . .
N4 C20 C19 121.0(19) . .
C21 C20 C19 123(2) . .
N5 C21 C22 117.7(19) . .
N5 C21 C20 120.2(14) . .
C22 C21 C20 122(2) . .
C23 C22 C21 118(2) . .
C24 C23 C22 126.0(19) . .
C23 C24 C25 111.5(16) . .
N5 C25 C24 125.5(16) . .
N6 C26 C27 177.5(16) . .
N7 C28 C29 178.6(15) . .
O4' Cl1 O3' 112.0(12) . .
O4' Cl1 O1' 112.5(12) . .
O3' Cl1 O1' 108.5(11) . .
O4' Cl1 O2 67.0(15) . .
O3' Cl1 O2 72.1(14) . .
O1' Cl1 O2 179.4(13) . .
O4' Cl1 O2' 109.6(12) . .
O3' Cl1 O2' 106.5(11) . .
O1' Cl1 O2' 107.4(11) . .
O2 Cl1 O2' 72.5(13) . .
O4' Cl1 O3 116.2(17) . .
O3' Cl1 O3 42.9(13) . .
O1' Cl1 O3 67.9(13) . .
O2 Cl1 O3 112.7(10) . .
O2' Cl1 O3 131.9(14) . .
O4' Cl1 O4 132.4(19) . .
O3' Cl1 O4 112.3(18) . .
O1' Cl1 O4 68.2(14) . .
O2 Cl1 O4 111.9(11) . .
O2' Cl1 O4 39.9(13) . .
O3 Cl1 O4 107.9(10) . .
O4' Cl1 O1 41.8(14) . .
O3' Cl1 O1 135.1(15) . .
O1' Cl1 O1 71.5(12) . .
O2 Cl1 O1 108.0(10) . .
O2' Cl1 O1 116.4(13) . .
O3 Cl1 O1 107.3(10) . .
O4 Cl1 O1 109.0(10) . .
O6 Cl2 O8 115.0(9) . .
O6 Cl2 O7 112.0(8) . .
O8 Cl2 O7 112.4(8) . .
O6 Cl2 O5 108.0(9) . .
O8 Cl2 O5 105.9(8) . .
O7 Cl2 O5 102.3(9) . .
C31 N8 C30 14(4) 2_565 .
C31 C30 C30 122(10) 2_565 2_565
C31 C30 N8 27(8) 2_565 .
C30 C30 N8 149(5) 2_565 .
C31 C30 C31 139(8) 2_565 .
C30 C30 C31 17(3) 2_565 .
N8 C30 C31 165(3) . .
C30 C31 N8 139(10) 2_565 2_565
C30 C31 C30 41(8) 2_565 .
N8 C31 C30 175(5) 2_565 .
C30 C31 C31 31(6) 2_565 2_565
N8 C31 C31 168(7) 2_565 2_565
C30 C31 C31 10(2) . 2_565
N9 C32 C33 158(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N6 2.183(12) .
Fe1 N7 2.184(12) .
Fe1 N2 2.254(10) .
Fe1 N3 2.255(10) .
Fe1 N4 2.271(11) .
Fe1 N5 2.284(11) .
Fe1 N1 2.351(10) .
N1 C5 1.335(14) .
N1 C1 1.350(16) .
N2 C6 1.304(14) .
N2 C10 1.330(16) .
N3 C15 1.316(17) .
N3 C11 1.355(16) .
N4 C20 1.300(18) .
N4 C16 1.323(17) .
N5 C25 1.265(16) .
N5 C21 1.369(18) .
N6 C26 1.135(18) .
N7 C28 1.123(15) .
C1 C2 1.360(18) .
C2 C3 1.362(19) .
C3 C4 1.37(2) .
C4 C5 1.395(18) .
C5 C6 1.493(18) .
C6 C7 1.411(17) .
C7 C8 1.33(2) .
C8 C9 1.36(2) .
C9 C10 1.385(19) .
C10 C11 1.448(19) .
C11 C12 1.40(2) .
C12 C13 1.42(3) .
C13 C14 1.31(2) .
C14 C15 1.37(2) .
C15 C16 1.44(2) .
C16 C17 1.34(2) .
C17 C18 1.43(3) .
C18 C19 1.33(3) .
C19 C20 1.43(2) .
C20 C21 1.41(2) .
C21 C22 1.40(2) .
C22 C23 1.36(2) .
C23 C24 1.35(2) .
C24 C25 1.434(19) .
C26 C27 1.53(2) .
C28 C29 1.54(2) .
Cl1 O4' 1.35(2) .
Cl1 O3' 1.38(2) .
Cl1 O1' 1.38(2) .
Cl1 O2 1.39(2) .
Cl1 O2' 1.40(2) .
Cl1 O3 1.412(19) .
Cl1 O4 1.42(2) .
Cl1 O1 1.447(17) .
Cl2 O6 1.337(13) .
Cl2 O8 1.337(13) .
Cl2 O7 1.396(12) .
Cl2 O5 1.442(13) .
N8 C31 0.97(5) 2_565
N8 C30 1.42(6) .
C30 C31 0.54(7) 2_565
C30 C30 1.20(6) 2_565
C30 C31 1.56(5) .
C31 C30 0.54(7) 2_565
C31 N8 0.97(5) 2_565
C31 C31 2.00(11) 2_565
N9 C32 1.18(3) .
C32 C33 1.39(3) .
