#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:20:45 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179056 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/18/4301803.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_4301803
loop_
_publ_author_name
'Jae Il Kim'
'Hyun Young Kwak'
'Jung Hee Yoon'
'Dae Won Ryu'
'In Young Yoo'
'Namgeun Yang'
'Beong Ki Cho'
'Je-Geun Park'
'Hyosug Lee'
'Chang Seop Hong'
_publ_section_title
;
Cyanide-Bridged FeIII-MnIII Bimetallic Complexes with Dimeric and Chain
Structures Constructed from a Newly Mademer-Fe Tricyanide: Structures and
Magnetic Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2956
_journal_page_last               2966
_journal_paper_doi               10.1021/ic802033q
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C46 H32 Fe N6 O P'
_chemical_formula_weight         771.60
_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                109.4130(10)
_cell_angle_beta                 97.306(2)
_cell_angle_gamma                100.320(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3047(4)
_cell_length_b                   14.7946(7)
_cell_length_c                   14.8284(7)
_cell_measurement_reflns_used    4331
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.271
_cell_volume                     1855.33(15)
_computing_cell_refinement       'Bruker SMART APEXll'
_computing_data_collection       'Bruker SMART APEXll'
_computing_data_reduction        SAINT
_computing_molecular_graphics    WingX
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.888
_diffrn_measured_fraction_theta_max 0.888
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19937
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.496
_exptl_absorpt_correction_T_max  0.9853
_exptl_absorpt_correction_T_min  0.9424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             798
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.649
_refine_diff_density_min         -1.498
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         8208
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1486
_refine_ls_R_factor_gt           0.1040
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0456P)²+10.4304P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2168
_refine_ls_wR_factor_ref         0.2432
_reflns_number_gt                5471
_reflns_number_total             8208
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802033q_si_001.cif
_cod_data_source_block           complex1
_cod_database_code               4301803
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 0.19618(12) 0.40789(6) 0.21154(6) 0.0556(3) Uani 1 1 d . . .
C1 C 0.2327(8) 0.4619(4) 0.3519(4) 0.0495(15) Uani 1 1 d . . .
N1 N 0.2577(9) 0.4932(5) 0.4358(4) 0.087(2) Uani 1 1 d . . .
C3 C 0.0847(7) 0.2860(4) 0.2208(4) 0.0432(13) Uani 1 1 d . . .
N3 N 0.0211(6) 0.2145(4) 0.2250(4) 0.0600(15) Uani 1 1 d . . .
C2 C 0.3002(7) 0.5403(4) 0.2227(4) 0.0419(13) Uani 1 1 d . . .
N2 N 0.3605(6) 0.6165(4) 0.2279(4) 0.0572(14) Uani 1 1 d . . .
N4 N 0.4008(8) 0.3651(5) 0.2331(5) 0.0745(18) Uani 1 1 d . . .
C4 C 0.4881(8) 0.3740(7) 0.3106(8) 0.084(3) Uani 1 1 d . . .
H4 H 0.4638 0.4082 0.3693 0.101 Uiso 1 1 calc R . .
C5 C 0.6162(8) 0.3382(6) 0.3170(7) 0.072(2) Uani 1 1 d . . .
H5 H 0.6694 0.3477 0.3782 0.087 Uiso 1 1 calc R . .
C6 C 0.6655(10) 0.2895(6) 0.2357(8) 0.088(3) Uani 1 1 d . . .
H6 H 0.7507 0.2650 0.2380 0.105 Uiso 1 1 calc R . .
C7 C 0.5647(11) 0.2789(5) 0.1385(9) 0.099(4) Uani 1 1 d . . .
C8 C 0.6117(12) 0.2360(6) 0.0646(12) 0.136(6) Uani 1 1 d . . .
H8 H 0.6960 0.2105 0.0634 0.163 Uiso 1 1 calc R . .
C9 C 0.5025(16) 0.2334(9) -0.0251(9) 0.120(4) Uani 1 1 d . . .
H9 H 0.5272 0.2059 -0.0856 0.144 Uiso 1 1 calc R . .
C10 C 0.3761(13) 0.2661(6) -0.0262(6) 0.086(3) Uani 1 1 d . . .
H10 H 0.3179 0.2598 -0.0848 0.104 Uiso 1 1 calc R . .
C11 C 0.3358(13) 0.3082(6) 0.0597(6) 0.094(3) Uani 1 1 d . . .
C12 C 0.4375(7) 0.3177(4) 0.1521(5) 0.0468(14) Uani 1 1 d . . .
N5 N 0.2285(8) 0.3447(4) 0.0804(6) 0.087(2) Uani 1 1 d . . .
C13 C 0.1073(8) 0.3404(4) 0.0073(4) 0.0467(15) Uani 1 1 d . . .
O1 O 0.0827(7) 0.3029(4) -0.0801(3) 0.0848(18) Uani 1 1 d . . .
C14 C 0.0003(11) 0.3925(5) 0.0581(6) 0.087(3) Uani 1 1 d . . .
C15 C -0.1352(13) 0.4031(7) -0.0099(7) 0.094(3) Uani 1 1 d . . .
H15 H -0.1442 0.3746 -0.0771 0.112 Uiso 1 1 calc R . .
C16 C -0.2349(16) 0.4494(7) 0.0225(7) 0.107(4) Uani 1 1 d . . .
H16 H -0.3125 0.4572 -0.0183 0.129 Uiso 1 1 calc R . .
C17 C -0.2120(10) 0.4918(7) 0.1382(11) 0.124(5) Uani 1 1 d . . .
C18 C -0.3126(11) 0.5326(8) 0.1599(13) 0.144(6) Uani 1 1 d . . .
H18 H -0.3874 0.5419 0.1184 0.172 Uiso 1 1 calc R . .
C19 C -0.2858(12) 0.5662(7) 0.2763(8) 0.092(3) Uani 1 1 d . . .
H19 H -0.3550 0.5982 0.3049 0.110 Uiso 1 1 calc R . .
C20 C -0.1770(9) 0.5551(6) 0.3400(8) 0.079(3) Uani 1 1 d . . .
H20 H -0.1733 0.5771 0.4069 0.095 Uiso 1 1 calc R . .
C21 C -0.0617(11) 0.5040(6) 0.2931(9) 0.113(4) Uani 1 1 d . . .
H21 H 0.0194 0.4929 0.3279 0.136 Uiso 1 1 calc R . .
C22 C -0.0956(7) 0.4740(4) 0.1840(5) 0.0460(14) Uani 1 1 d . . .
N6 N 0.0183(8) 0.4246(5) 0.1437(6) 0.084(2) Uani 1 1 d . . .
P1 P 0.37076(17) 0.99143(10) 0.29852(10) 0.0370(3) Uani 1 1 d . . .
C23 C 0.2522(6) 0.9152(4) 0.3454(4) 0.0373(12) Uani 1 1 d . . .
C24 C 0.2086(7) 0.8122(4) 0.2952(5) 0.0515(15) Uani 1 1 d . . .
H24 H 0.2424 0.7830 0.2386 0.062 Uiso 1 1 calc R . .
C25 C 0.1148(8) 0.7552(5) 0.3314(5) 0.0578(17) Uani 1 1 d . . .
H25 H 0.0847 0.6873 0.2985 0.069 Uiso 1 1 calc R . .
C26 C 0.0659(8) 0.7982(5) 0.4152(5) 0.0617(18) Uani 1 1 d . . .
H26 H 0.0030 0.7592 0.4390 0.074 Uiso 1 1 calc R . .
C27 C 0.1094(7) 0.8986(5) 0.4644(5) 0.0547(16) Uani 1 1 d . . .
H27 H 0.0758 0.9272 0.5213 0.066 Uiso 1 1 calc R . .
C28 C 0.2030(7) 0.9573(4) 0.4296(4) 0.0441(13) Uani 1 1 d . . .
H28 H 0.2325 1.0251 0.4632 0.053 Uiso 1 1 calc R . .
C29 C 0.2818(6) 0.9776(4) 0.1776(4) 0.0387(12) Uani 1 1 d . . .
C30 C 0.3476(9) 1.0410(6) 0.1353(5) 0.078(3) Uani 1 1 d . . .
H30 H 0.4322 1.0907 0.1705 0.094 Uiso 1 1 calc R . .
C31 C 0.2885(10) 1.0309(6) 0.0420(6) 0.081(3) Uani 1 1 d . . .
H31 H 0.3333 1.0734 0.0141 0.098 Uiso 1 1 calc R . .
C32 C 0.1644(8) 0.9586(5) -0.0100(5) 0.0568(17) Uani 1 1 d . . .
H32 H 0.1252 0.9512 -0.0736 0.068 Uiso 1 1 calc R . .
C33 C 0.0981(8) 0.8975(5) 0.0315(5) 0.0581(17) Uani 1 1 d . . .
H33 H 0.0124 0.8490 -0.0039 0.070 Uiso 1 1 calc R . .
C34 C 0.1556(7) 0.9061(4) 0.1253(4) 0.0461(14) Uani 1 1 d . . .
H34 H 0.1090 0.8637 0.1528 0.055 Uiso 1 1 calc R . .
C35 C 0.5478(6) 0.9601(4) 0.2943(4) 0.0384(12) Uani 1 1 d . . .
C36 C 0.6617(8) 1.0204(5) 0.2729(5) 0.0601(17) Uani 1 1 d . . .
H36 H 0.6467 1.0782 0.2654 0.072 Uiso 1 1 calc R . .
C37 C 0.7966(8) 0.9952(7) 0.2629(5) 0.070(2) Uani 1 1 d . . .
H37 H 0.8718 1.0353 0.2482 0.084 Uiso 1 1 calc R . .
C38 C 0.8178(8) 0.9107(6) 0.2749(5) 0.069(2) Uani 1 1 d . . .
H38 H 0.9078 0.8931 0.2674 0.083 Uiso 1 1 calc R . .
C39 C 0.7103(9) 0.8516(6) 0.2976(6) 0.067(2) Uani 1 1 d . . .
H39 H 0.7277 0.7949 0.3065 0.081 Uiso 1 1 calc R . .
C40 C 0.5751(7) 0.8761(5) 0.3076(5) 0.0517(15) Uani 1 1 d . . .
H40 H 0.5018 0.8357 0.3233 0.062 Uiso 1 1 calc R . .
C41 C 0.3973(6) 1.1169(4) 0.3777(4) 0.0398(12) Uani 1 1 d . . .
C42 C 0.2856(7) 1.1659(4) 0.3652(4) 0.0472(14) Uani 1 1 d . . .
H42 H 0.2038 1.1354 0.3138 0.057 Uiso 1 1 calc R . .
C43 C 0.2982(8) 1.2602(4) 0.4301(5) 0.0554(16) Uani 1 1 d . . .
H43 H 0.2233 1.2928 0.4231 0.067 Uiso 1 1 calc R . .
C44 C 0.4204(9) 1.3064(5) 0.5051(5) 0.0600(18) Uani 1 1 d . . .
H44 H 0.4284 1.3703 0.5478 0.072 Uiso 1 1 calc R . .
C45 C 0.5311(8) 1.2583(5) 0.5172(5) 0.0586(17) Uani 1 1 d . . .
H45 H 0.6133 1.2898 0.5682 0.070 Uiso 1 1 calc R . .
C46 C 0.5202(7) 1.1627(4) 0.4534(4) 0.0493(15) Uani 1 1 d . . .
H46 H 0.5946 1.1301 0.4616 0.059 Uiso 1 1 calc 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'
P P 0.1023 0.0942 '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
N6 Fe1 C1 116.6(3) . . ?
N6 Fe1 N5 83.7(4) . . ?
C1 Fe1 N5 159.6(3) . . ?
N6 Fe1 C2 89.2(2) . . ?
C1 Fe1 C2 85.2(2) . . ?
N5 Fe1 C2 93.8(2) . . ?
N6 Fe1 C3 91.1(2) . . ?
C1 Fe1 C3 86.5(2) . . ?
N5 Fe1 C3 95.3(2) . . ?
C2 Fe1 C3 170.8(2) . . ?
N6 Fe1 N4 159.1(3) . . ?
C1 Fe1 N4 84.3(3) . . ?
N5 Fe1 N4 75.4(3) . . ?
C2 Fe1 N4 92.1(2) . . ?
C3 Fe1 N4 90.9(2) . . ?
N1 C1 Fe1 178.3(7) . . ?
N3 C3 Fe1 178.9(6) . . ?
N2 C2 Fe1 179.1(5) . . ?
C4 N4 C12 115.3(8) . . ?
C4 N4 Fe1 131.5(7) . . ?
C12 N4 Fe1 113.1(5) . . ?
N4 C4 C5 127.2(10) . . ?
C6 C5 C4 121.7(9) . . ?
C5 C6 C7 113.3(8) . . ?
C8 C7 C12 133.2(13) . . ?
C8 C7 C6 113.0(12) . . ?
C12 C7 C6 113.7(8) . . ?
C7 C8 C9 106.9(11) . . ?
C10 C9 C8 128.0(12) . . ?
C9 C10 C11 118.6(12) . . ?
N5 C11 C10 132.5(12) . . ?
N5 C11 C12 109.8(7) . . ?
C10 C11 C12 117.7(11) . . ?
N4 C12 C7 128.6(8) . . ?
N4 C12 C11 115.7(7) . . ?
C7 C12 C11 115.5(8) . . ?
C11 N5 C13 122.6(8) . . ?
C11 N5 Fe1 125.8(8) . . ?
C13 N5 Fe1 111.6(5) . . ?
O1 C13 N5 131.3(7) . . ?
O1 C13 C14 120.7(7) . . ?
N5 C13 C14 108.0(6) . . ?
N6 C14 C13 121.5(10) . . ?
N6 C14 C15 122.5(10) . . ?
C13 C14 C15 116.0(7) . . ?
C16 C15 C14 123.8(10) . . ?
C15 C16 C17 113.8(11) . . ?
C18 C17 C22 137.4(16) . . ?
C18 C17 C16 107.9(12) . . ?
C22 C17 C16 114.6(12) . . ?
C17 C18 C19 104.0(12) . . ?
C20 C19 C18 130.0(9) . . ?
C19 C20 C21 115.0(10) . . ?
C22 C21 C20 111.7(9) . . ?
C17 C22 N6 129.4(9) . . ?
C17 C22 C21 121.8(10) . . ?
N6 C22 C21 108.9(7) . . ?
C14 N6 C22 115.8(8) . . ?
C14 N6 Fe1 115.1(8) . . ?
C22 N6 Fe1 129.1(6) . . ?
C41 P1 C35 109.7(3) . . ?
C41 P1 C23 107.7(3) . . ?
C35 P1 C23 111.2(3) . . ?
C41 P1 C29 108.8(2) . . ?
C35 P1 C29 109.4(3) . . ?
C23 P1 C29 110.0(3) . . ?
C28 C23 C24 119.9(5) . . ?
C28 C23 P1 120.1(4) . . ?
C24 C23 P1 120.0(4) . . ?
C25 C24 C23 119.1(6) . . ?
C26 C25 C24 120.5(6) . . ?
C25 C26 C27 120.3(6) . . ?
C26 C27 C28 120.3(6) . . ?
C23 C28 C27 119.9(6) . . ?
C34 C29 C30 119.0(6) . . ?
C34 C29 P1 123.0(4) . . ?
C30 C29 P1 117.9(5) . . ?
C31 C30 C29 120.3(6) . . ?
C32 C31 C30 120.3(7) . . ?
C33 C32 C31 119.7(6) . . ?
C32 C33 C34 121.2(6) . . ?
C29 C34 C33 119.5(6) . . ?
C40 C35 C36 118.1(6) . . ?
C40 C35 P1 122.6(5) . . ?
C36 C35 P1 119.2(5) . . ?
C37 C36 C35 120.8(7) . . ?
C38 C37 C36 119.0(7) . . ?
C39 C38 C37 121.5(7) . . ?
C38 C39 C40 119.8(7) . . ?
C39 C40 C35 120.6(6) . . ?
C46 C41 C42 120.5(5) . . ?
C46 C41 P1 121.3(4) . . ?
C42 C41 P1 118.1(4) . . ?
C43 C42 C41 119.2(6) . . ?
C44 C43 C42 120.6(6) . . ?
C43 C44 C45 120.2(6) . . ?
C44 C45 C46 120.2(6) . . ?
C41 C46 C45 119.2(6) . . ?
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 N6 1.923(7) . ?
Fe1 C1 1.924(6) . ?
Fe1 N5 1.945(8) . ?
Fe1 C2 1.966(6) . ?
Fe1 C3 1.969(6) . ?
Fe1 N4 2.130(7) . ?
C1 N1 1.149(8) . ?
C3 N3 1.141(7) . ?
C2 N2 1.139(7) . ?
N4 C4 1.273(10) . ?
N4 C12 1.298(8) . ?
C4 C5 1.393(10) . ?
C5 C6 1.366(12) . ?
C6 C7 1.562(14) . ?
C7 C8 1.247(13) . ?
C7 C12 1.413(11) . ?
C8 C9 1.553(17) . ?
C9 C10 1.350(15) . ?
C10 C11 1.352(10) . ?
C11 N5 1.243(12) . ?
C11 C12 1.512(12) . ?
N5 C13 1.439(10) . ?
C13 O1 1.200(7) . ?
C13 C14 1.494(12) . ?
C14 N6 1.177(10) . ?
C14 C15 1.576(14) . ?
C15 C16 1.297(15) . ?
C16 C17 1.590(16) . ?
C17 C18 1.222(14) . ?
C17 C22 1.319(10) . ?
C18 C19 1.600(17) . ?
C19 C20 1.365(13) . ?
C20 C21 1.528(13) . ?
C21 C22 1.502(13) . ?
C22 N6 1.471(10) . ?
P1 C41 1.789(5) . ?
P1 C35 1.792(6) . ?
P1 C23 1.800(5) . ?
P1 C29 1.806(6) . ?
C23 C28 1.374(8) . ?
C23 C24 1.410(7) . ?
C24 C25 1.384(8) . ?
C25 C26 1.371(9) . ?
C26 C27 1.376(9) . ?
C27 C28 1.386(9) . ?
C29 C34 1.370(8) . ?
C29 C30 1.390(8) . ?
C30 C31 1.370(9) . ?
C31 C32 1.362(10) . ?
C32 C33 1.358(9) . ?
C33 C34 1.380(8) . ?
C35 C40 1.383(8) . ?
C35 C36 1.398(8) . ?
C36 C37 1.384(10) . ?
C37 C38 1.365(11) . ?
C38 C39 1.358(11) . ?
C39 C40 1.382(9) . ?
C41 C46 1.384(8) . ?
C41 C42 1.396(8) . ?
C42 C43 1.381(8) . ?
C43 C44 1.375(9) . ?
C44 C45 1.378(10) . ?
C45 C46 1.393(8) . ?
