#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:58:33 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202018 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/17/8101744.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_8101744
loop_
_publ_author_name
'Feng, Y.-L.'
_publ_section_title
;
Crystal structure of bis(1,10-phenanthroline-1\kN,\kN')-tetrachloro-
1\kCl,2κ³Cl-μ-oxo-1:2κ²O-diiron(III) trichloromethane solvate, 
[FeCl(C₁₂H₈N₄)₂]O(FeCl₃) · CHCl₃, a dinuclear iron(III) 
complex with an unsymmetrical μ-oxo bridge
;
_journal_issue                   2
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              201
_journal_page_last               202
_journal_volume                  220
_journal_year                    2005
_chemical_formula_sum            'C25 H17 Cl7 Fe2 N4 O'
_chemical_formula_weight         749.28
_chemical_name_systematic
;
tetrachloro-bis(1,10-phenanthroline-N,N')(μ-oxo)diiron(III) trichloromethane 
solvate
;
_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                94.26(3)
_cell_angle_beta                 93.87(3)
_cell_angle_gamma                98.53(3)
_cell_formula_units_Z            2
_cell_length_a                   8.0140(16)
_cell_length_b                   11.822(2)
_cell_length_c                   15.795(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1471.1(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID IP'
_diffrn_measurement_method       omega
_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  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10026
_diffrn_reflns_theta_full        27.39
_diffrn_reflns_theta_max         27.39
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    1.650
_exptl_absorpt_correction_T_max  0.8524
_exptl_absorpt_correction_T_min  0.4926
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.770
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         6253
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0659
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0734P)²+4.0758P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1642
_refine_ls_wR_factor_ref         0.1714
_reflns_number_gt                5311
_reflns_number_total             6253
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-1485.cff
_cod_data_source_block           Fe(III)2OCl4phen2
_cod_original_cell_volume        1471.0(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               8101744
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_Wyckoff_symbol
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.46877(8) 0.18113(5) 0.31672(4) 0.03358(17) Uani 1 2 i d . . .
Fe2 Fe 0.41768(9) -0.10035(6) 0.23509(5) 0.0473(2) Uani 1 2 i d . . .
Cl1 Cl 0.74142(15) 0.24723(10) 0.37651(8) 0.0472(3) Uani 1 2 i d . . .
Cl2 Cl 0.2034(3) -0.18491(17) 0.3028(2) 0.1298(12) Uani 1 2 i d . . .
Cl3 Cl 0.6085(2) -0.21860(12) 0.23161(9) 0.0597(3) Uani 1 2 i d . . .
Cl4 Cl 0.3468(4) -0.0743(2) 0.10115(13) 0.1234(11) Uani 1 2 i d . . .
Cl5 Cl 1.0336(3) 0.4443(3) 0.24837(19) 0.1274(10) Uani 1 2 i d . . .
Cl6 Cl 1.2423(7) 0.4925(3) 0.1166(2) 0.1830(18) Uani 1 2 i d . . .
Cl7 Cl 0.9472(9) 0.5999(4) 0.1290(5) 0.314(5) Uani 1 2 i d . . .
O1 O 0.4917(4) 0.0325(3) 0.2913(2) 0.0409(7) Uani 1 2 i d . . .
N1 N 0.5038(5) 0.2401(3) 0.1923(2) 0.0411(8) Uani 1 2 i d . . .
N2 N 0.2077(5) 0.1515(3) 0.2498(2) 0.0398(8) Uani 1 2 i d . . .
N3 N 0.4066(5) 0.3543(3) 0.3613(2) 0.0368(7) Uani 1 2 i d . . .
N4 N 0.3457(5) 0.1541(3) 0.4315(2) 0.0356(7) Uani 1 2 i d . . .
C1 C 0.6492(7) 0.2851(5) 0.1660(4) 0.0557(13) Uani 1 2 i d . . .
H1 H 0.7462 0.3024 0.2065 0.067 Uiso 1 2 i d R . .
C2 C 0.6657(9) 0.3080(6) 0.0803(4) 0.0687(17) Uani 1 2 i d . . .
H2 H 0.7742 0.3400 0.0632 0.082 Uiso 1 2 i d R . .
C3 C 0.5310(9) 0.2839(5) 0.0229(4) 0.0650(16) Uani 1 2 i d . . .
H3 H 0.5422 0.3015 -0.0350 0.078 Uiso 1 2 i d R . .
C4 C 0.3718(8) 0.2343(5) 0.0491(3) 0.0541(13) Uani 1 2 i d . . .
C5 C 0.2231(10) 0.2023(6) -0.0079(4) 0.0686(17) Uani 1 2 i d . . .
H5 H 0.2275 0.2152 -0.0671 0.082 Uiso 1 2 i d R . .
C6 C 0.0770(9) 0.1563(6) 0.0209(4) 0.0673(16) Uani 1 2 i d . . .
H6 H -0.0214 0.1339 -0.0183 0.081 Uiso 1 2 i d R . .
C7 C 0.0618(7) 0.1376(5) 0.1081(3) 0.0553(13) Uani 1 2 i d . . .
C8 C -0.0866(7) 0.0866(5) 0.1416(4) 0.0607(14) Uani 1 2 i d . . .
H8 H -0.1868 0.0604 0.1044 0.073 Uiso 1 2 i d R . .
C9 C -0.0854(7) 0.0706(6) 0.2257(4) 0.0644(15) Uani 1 2 i d . . .
H9 H -0.1874 0.0383 0.2491 0.077 Uiso 1 2 i d R . .
C10 C 0.0624(6) 0.1041(5) 0.2784(3) 0.0502(11) Uani 1 2 i d . . .
H10 H 0.0615 0.0911 0.3377 0.060 Uiso 1 2 i d R . .
C11 C 0.2089(6) 0.1677(4) 0.1659(3) 0.0411(9) Uani 1 2 i d . . .
C12 C 0.3656(6) 0.2166(4) 0.1352(3) 0.0426(10) Uani 1 2 i d . . .
C13 C 0.4511(6) 0.4549(4) 0.3302(3) 0.0439(10) Uani 1 2 i d . . .
H13 H 0.5160 0.4579 0.2812 0.053 Uiso 1 2 i d R . .
C14 C 0.4072(7) 0.5566(4) 0.3660(3) 0.0488(11) Uani 1 2 i d . . .
H14 H 0.4412 0.6275 0.3414 0.059 Uiso 1 2 i d R . .
C15 C 0.3139(6) 0.5556(4) 0.4347(3) 0.0457(10) Uani 1 2 i d . . .
H15 H 0.2826 0.6256 0.4590 0.055 Uiso 1 2 i d R . .
C16 C 0.2662(6) 0.4508(4) 0.4705(3) 0.0387(9) Uani 1 2 i d . . .
C17 C 0.1720(6) 0.4392(4) 0.5448(3) 0.0468(11) Uani 1 2 i d . . .
H17 H 0.1357 0.5059 0.5716 0.056 Uiso 1 2 i d R . .
C18 C 0.1368(6) 0.3388(5) 0.5778(3) 0.0483(11) Uani 1 2 i d . . .
H18 H 0.0706 0.3337 0.6262 0.058 Uiso 1 2 i d R . .
C19 C 0.1943(6) 0.2373(4) 0.5412(3) 0.0407(9) Uani 1 2 i d . . .
C20 C 0.1676(6) 0.1299(5) 0.5759(3) 0.0468(11) Uani 1 2 i d . . .
H20 H 0.1067 0.1210 0.6258 0.056 Uiso 1 2 i d R . .
C21 C 0.2301(7) 0.0380(4) 0.5382(3) 0.0493(11) Uani 1 2 i d . . .
H21 H 0.2130 -0.0357 0.5607 0.059 Uiso 1 2 i d R . .
C22 C 0.3182(6) 0.0545(4) 0.4651(3) 0.0419(10) Uani 1 2 i d . . .
H22 H 0.3616 -0.0095 0.4382 0.050 Uiso 1 2 i d R . .
C23 C 0.2842(5) 0.2450(4) 0.4685(2) 0.0331(8) Uani 1 2 i d . . .
C24 C 0.3180(5) 0.3530(4) 0.4314(3) 0.0342(8) Uani 1 2 i d . . .
C25 C 1.1076(14) 0.5519(7) 0.1807(6) 0.112(3) Uani 1 2 i d . . .
H25 H 1.1735 0.6148 0.2157 0.134 Uiso 1 2 i d R . .
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
O1 Fe1 N4 96.16(14) . . ?
O1 Fe1 N1 97.88(15) . . ?
N4 Fe1 N1 156.97(14) . . ?
O1 Fe1 N2 91.03(14) . . ?
N4 Fe1 N2 86.25(14) . . ?
N1 Fe1 N2 75.36(15) . . ?
O1 Fe1 N3 170.67(14) . . ?
N4 Fe1 N3 75.16(13) . . ?
N1 Fe1 N3 89.35(14) . . ?
N2 Fe1 N3 85.08(14) . . ?
O1 Fe1 Cl1 98.32(11) . . ?
N4 Fe1 Cl1 98.82(11) . . ?
N1 Fe1 Cl1 97.10(12) . . ?
N2 Fe1 Cl1 168.78(11) . . ?
N3 Fe1 Cl1 86.56(10) . . ?
O1 Fe2 Cl4 109.39(13) . . ?
O1 Fe2 Cl3 113.73(12) . . ?
Cl4 Fe2 Cl3 106.27(8) . . ?
O1 Fe2 Cl2 107.12(12) . . ?
Cl4 Fe2 Cl2 113.75(14) . . ?
Cl3 Fe2 Cl2 106.71(9) . . ?
Fe2 O1 Fe1 149.5(2) . . ?
C1 N1 C12 118.8(4) . . ?
C1 N1 Fe1 125.2(4) . . ?
C12 N1 Fe1 115.6(3) . . ?
C10 N2 C11 118.0(4) . . ?
C10 N2 Fe1 128.4(3) . . ?
C11 N2 Fe1 112.6(3) . . ?
C13 N3 C24 117.7(4) . . ?
C13 N3 Fe1 128.7(3) . . ?
C24 N3 Fe1 113.6(3) . . ?
C22 N4 C23 118.7(4) . . ?
C22 N4 Fe1 124.5(3) . . ?
C23 N4 Fe1 116.6(3) . . ?
N1 C1 C2 121.7(6) . . ?
N1 C1 H1 118.6 . . ?
C2 C1 H1 119.7 . . ?
C3 C2 C1 120.2(6) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 119.4 . . ?
C2 C3 C4 119.5(5) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 120.6 . . ?
C12 C4 C3 116.6(5) . . ?
C12 C4 C5 119.9(6) . . ?
C3 C4 C5 123.4(5) . . ?
C6 C5 C4 120.5(5) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.7 . . ?
C5 C6 C7 122.3(6) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 H6 118.1 . . ?
C8 C7 C6 124.8(5) . . ?
C8 C7 C11 116.9(5) . . ?
C6 C7 C11 118.2(6) . . ?
C9 C8 C7 119.8(5) . . ?
C9 C8 H8 120.4 . . ?
C7 C8 H8 119.8 . . ?
C8 C9 C10 120.0(6) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
N2 C10 C9 122.7(5) . . ?
N2 C10 H10 118.3 . . ?
C9 C10 H10 118.9 . . ?
N2 C11 C7 122.5(5) . . ?
N2 C11 C12 117.8(4) . . ?
C7 C11 C12 119.7(4) . . ?
N1 C12 C4 123.1(5) . . ?
N1 C12 C11 117.4(4) . . ?
C4 C12 C11 119.4(5) . . ?
N3 C13 C14 122.4(4) . . ?
N3 C13 H13 119.0 . . ?
C14 C13 H13 118.6 . . ?
C15 C14 C13 120.3(4) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.9 . . ?
C14 C15 C16 119.1(4) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.7 . . ?
C24 C16 C15 116.9(4) . . ?
C24 C16 C17 118.7(4) . . ?
C15 C16 C17 124.4(4) . . ?
C18 C17 C16 121.6(4) . . ?
C18 C17 H17 119.4 . . ?
C16 C17 H17 119.0 . . ?
C17 C18 C19 121.1(4) . . ?
C17 C18 H18 119.3 . . ?
C19 C18 H18 119.6 . . ?
C23 C19 C20 117.7(4) . . ?
C23 C19 C18 118.8(4) . . ?
C20 C19 C18 123.5(4) . . ?
C21 C20 C19 119.8(4) . . ?
C21 C20 H20 119.9 . . ?
C19 C20 H20 120.3 . . ?
C20 C21 C22 118.2(4) . . ?
C20 C21 H21 121.1 . . ?
C22 C21 H21 120.7 . . ?
N4 C22 C21 123.3(4) . . ?
N4 C22 H22 118.1 . . ?
C21 C22 H22 118.6 . . ?
N4 C23 C19 122.3(4) . . ?
N4 C23 C24 117.7(4) . . ?
C19 C23 C24 120.0(4) . . ?
N3 C24 C16 123.5(4) . . ?
N3 C24 C23 116.7(4) . . ?
C16 C24 C23 119.7(4) . . ?
Cl7 C25 Cl6 115.0(6) . . ?
Cl7 C25 Cl5 111.5(7) . . ?
Cl6 C25 Cl5 106.0(5) . . ?
Cl7 C25 H25 108.7 . . ?
Cl6 C25 H25 107.5 . . ?
Cl5 C25 H25 107.9 . . ?
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 1.812(3) . ?
Fe1 N4 2.143(4) . ?
Fe1 N1 2.156(4) . ?
Fe1 N2 2.247(4) . ?
Fe1 N3 2.251(4) . ?
Fe1 Cl1 2.3200(15) . ?
Fe2 O1 1.747(3) . ?
Fe2 Cl4 2.209(2) . ?
Fe2 Cl3 2.2207(15) . ?
Fe2 Cl2 2.234(2) . ?
Cl5 C25 1.782(11) . ?
Cl6 C25 1.718(11) . ?
Cl7 C25 1.669(9) . ?
N1 C1 1.314(6) . ?
N1 C12 1.362(6) . ?
N2 C10 1.338(6) . ?
N2 C11 1.353(6) . ?
N3 C13 1.330(6) . ?
N3 C24 1.356(5) . ?
N4 C22 1.323(6) . ?
N4 C23 1.358(5) . ?
C1 C2 1.412(8) . ?
C1 H1 0.9600 . ?
C2 C3 1.344(9) . ?
C2 H2 0.9600 . ?
C3 C4 1.424(9) . ?
C3 H3 0.9599 . ?
C4 C12 1.394(7) . ?
C4 C5 1.431(9) . ?
C5 C6 1.339(10) . ?
C5 H5 0.9601 . ?
C6 C7 1.422(8) . ?
C6 H6 0.9601 . ?
C7 C8 1.406(9) . ?
C7 C11 1.425(7) . ?
C8 C9 1.354(9) . ?
C8 H8 0.9600 . ?
C9 C10 1.390(8) . ?
C9 H9 0.9600 . ?
C10 H10 0.9600 . ?
C11 C12 1.434(7) . ?
C13 C14 1.393(7) . ?
C13 H13 0.9600 . ?
C14 C15 1.358(7) . ?
C14 H14 0.9600 . ?
C15 C16 1.413(7) . ?
C15 H15 0.9600 . ?
C16 C24 1.400(6) . ?
C16 C17 1.442(6) . ?
C17 C18 1.331(7) . ?
C17 H17 0.9600 . ?
C18 C19 1.444(7) . ?
C18 H18 0.9600 . ?
C19 C23 1.398(6) . ?
C19 C20 1.413(7) . ?
C20 C21 1.375(7) . ?
C20 H20 0.9600 . ?
C21 C22 1.404(6) . ?
C21 H21 0.9600 . ?
C22 H22 0.9600 . ?
C23 C24 1.441(6) . ?
C25 H25 0.9600 . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30653875
