#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/30/4323025.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_4323025
loop_
_publ_author_name
'Hitoshi Miyasaka'
'Hisashi Okawa'
'Akira Miyazaki'
'Toshiaki Enoki'
_publ_section_title
;
 Synthesis, Crystal and Network Structures, and Magnetic Properties of a
 Hybrid Layered Compound: [K(18-cr)(2-PrOH)2][{Mn(acacen)}2{Fe(CN)6}]
 (18-cr = 18-Crown-6-ether, acacen
 =N,N'-Ethylenebis(acetylacetonylideneiminate))
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4878
_journal_page_last               4883
_journal_paper_doi               10.1021/ic980448p
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C42 H64 Fe K Mn2 N10 O12'
_chemical_formula_weight         1105.85
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_audit_creation_date             'Fri Nov  7 17:13:29 1997'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 105.64(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2.00
_cell_length_a                   13.272(3)
_cell_length_b                   15.768(2)
_cell_length_c                   14.771(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    23.0
_cell_measurement_theta_max      30.01
_cell_measurement_theta_min      29.86
_cell_volume                     2976.7(9)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan: PROCESS (MSC)'
_computing_publication_material  'teXsan: FINISH (MSC)'
_computing_structure_refinement  'teXsan: LS (MSC)'
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      23.0
_diffrn_measurement_device       AFC7R
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  4.53
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -2
_diffrn_reflns_theta_max         27.5128
_diffrn_standards_decay_%        -0.60
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.851
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.678
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       prismatic
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.350
_refine_diff_density_max         0.72150
_refine_diff_density_min         -0.58030
_refine_ls_extinction_coef       5.93795
_refine_ls_extinction_method     Zachariasen_type_2_Gaussian_isotropic
_refine_ls_goodness_of_fit_obs   4.050
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         5291
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0560
_refine_ls_shift/esd_max         0.2480
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_obs         0.0550
_reflns_number_observed          5291
_reflns_number_total             7401
_cod_data_source_file            ic980448p.cif
_cod_data_source_block           K(cr)Mn(acacen)Fe(CN)
_cod_original_sg_symbol_H-M      'P 21/a '
_cod_original_formula_sum        C42H64O12N10KMn2Fe1
_cod_database_code               4323025
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'1/2-x,1/2+y,   -z'
'   -x,   -y,   -z'
'1/2+x,1/2-y,   +z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
Fe 0.5000 0.0000 0.5000 0.0298 Uij ? ?
Mn 0.17368(4) 0.19034(4) 0.49355(5) 0.0491 Uij ? ?
K 0.5000 0.0000 0.0000 0.0606 Uij ? ?
O1 0.1415(2) 0.1808(2) 0.6101(2) 0.0604 Uij ? ?
O2 0.0599(2) 0.1188(2) 0.4363(2) 0.0575 Uij ? ?
O3 0.5256(4) 0.1617(3) 0.0937(4) 0.1134 Uij ? ?
O4 0.5862(3) 0.0117(3) 0.1852(2) 0.0986 Uij ? ?
O5 0.5954(4) -0.1436(3) 0.0967(4) 0.1153 Uij ? ?
O6 0.3385(3) -0.0224(4) 0.0861(2) 0.1278 Uij ? ?
N1 0.2824(3) 0.2742(3) 0.5415(5) 0.1073 Uij ? ?
N2 0.2131(4) 0.2031(4) 0.3750(5) 0.1052 Uij ? ?
N3 0.2948(2) 0.0798(2) 0.5226(2) 0.0459 Uij ? ?
N4 0.5665(2) 0.1818(2) 0.4615(3) 0.0555 Uij ? ?
N5 0.3887(3) -0.0140(2) 0.2868(2) 0.0604 Uij ? ?
C1 0.1152(8) 0.2192(6) 0.7543(5) 0.1730 Uij ? ?
C2 0.1673(5) 0.2356(4) 0.6778(4) 0.0936 Uij ? ?
C3 0.2342(7) 0.3010(5) 0.6800(6) 0.1430 Uij ? ?
C4 0.2886(5) 0.3206(4) 0.6174(9) 0.1528 Uij ? ?
C5 0.3578(6) 0.3990(4) 0.635(1) 0.2657 Uij ? ?
C6 0.3396(10) 0.2927(7) 0.473(1) 0.2803 Uij ? ?
C7 0.3108(5) 0.2567(9) 0.3934(9) 0.2307 Uij ? ?
C8 0.218(1) 0.1719(7) 0.2142(7) 0.2763 Uij ? ?
C9 0.172(1) 0.1657(7) 0.2974(8) 0.1817 Uij ? ?
C10 0.085(1) 0.1161(6) 0.2860(5) 0.1509 Uij ? ?
C11 0.0316(5) 0.0944(3) 0.3490(4) 0.0889 Uij ? ?
C12 -0.0635(5) 0.0387(4) 0.3267(6) 0.1510 Uij ? ?
C13 0.3710(2) 0.0484(2) 0.5161(2) 0.0348 Uij ? ?
C14 0.5435(2) 0.1143(2) 0.4759(2) 0.0386 Uij ? ?
C15 0.4302(3) -0.0107(2) 0.3659(2) 0.0410 Uij ? ?
C16 0.5239(7) 0.1459(5) 0.1906(7) 0.1361 Uij ? ?
C17 0.6071(7) 0.0868(8) 0.2335(5) 0.1480 Uij ? ?
C18 0.6415(6) -0.0603(8) 0.2326(4) 0.1470 Uij ? ?
C19 0.5883(6) -0.1359(7) 0.1892(8) 0.1532 Uij ? ?
C20 0.5510(8) -0.2208(6) 0.051(1) 0.1747 Uij ? ?
C21 0.557(1) -0.2157(6) -0.0475(10) 0.1802 Uij ? ?
C22 0.2422(6) -0.0590(8) 0.0484(5) 0.1521 Uij ? ?
C23 0.177(1) -0.006(2) 0.049(2) 0.5502 Uij ? ?
C24 0.221(1) -0.073(2) -0.0446(8) 0.3710 Uij ? ?
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0 84 0.003 0.002 'International Tables'
H 0 128 0.000 0.000 'International Tables'
O 0 24 0.011 0.006 'International Tables'
N 0 20 0.006 0.003 'International Tables'
K 0 2 0.200 0.250 'International Tables'
Mn 0 4 0.337 0.728 'International Tables'
Fe 0 2 0.346 0.844 'International Tables'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
? ? ?
? ? ?
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C(13) Fe C(13) 180.0000 ? ? ? yes
C(13) Fe C(14) 88.5(1) ? ? ? yes
C(13) Fe C(14) 91.5(1) ? ? ? yes
C(13) Fe C(15) 88.0(1) ? ? ? yes
C(13) Fe C(15) 92.0(1) ? ? ? yes
C(13) Fe C(14) 91.5(1) ? ? ? yes
C(13) Fe C(14) 88.5(1) ? ? ? yes
C(13) Fe C(15) 92.0(1) ? ? ? yes
C(13) Fe C(15) 88.0(1) ? ? ? yes
C(14) Fe C(14) 180.0000 ? ? ? yes
C(14) Fe C(15) 88.7(1) ? ? ? yes
C(14) Fe C(15) 91.3(1) ? ? ? yes
C(14) Fe C(15) 91.3(1) ? ? ? yes
C(14) Fe C(15) 88.7(1) ? ? ? yes
C(15) Fe C(15) 180.0000 ? ? ? yes
O(1) Mn O(2) 90.6(1) ? ? ? yes
O(1) Mn N(1) 92.9(2) ? ? ? yes
O(1) Mn N(2) 177.4(2) ? ? ? yes
O(1) Mn N(3) 95.0(1) ? ? ? yes
O(1) Mn N(4) 88.8(1) ? ? ? yes
O(2) Mn N(1) 173.1(2) ? ? ? yes
O(2) Mn N(2) 92.0(2) ? ? ? yes
O(2) Mn N(3) 93.7(1) ? ? ? yes
O(2) Mn N(4) 93.0(1) ? ? ? yes
N(1) Mn N(2) 84.6(3) ? ? ? yes
N(1) Mn N(3) 92.0(1) ? ? ? yes
N(1) Mn N(4) 81.1(1) ? ? ? yes
N(2) Mn N(3) 84.5(1) ? ? ? yes
N(2) Mn N(4) 91.4(2) ? ? ? yes
N(3) Mn N(4) 172.3(1) ? ? ? yes
O(3) K O(3) 180.0000 ? ? ? yes
O(3) K O(4) 58.9(2) ? ? ? yes
O(3) K O(4) 121.1(2) ? ? ? yes
O(3) K O(5) 119.6(2) ? ? ? yes
O(3) K O(5) 60.4(2) ? ? ? yes
O(3) K O(6) 84.2(1) ? ? ? yes
O(3) K O(6) 95.8(1) ? ? ? yes
O(3) K O(4) 121.1(2) ? ? ? yes
O(3) K O(4) 58.9(2) ? ? ? yes
O(3) K O(5) 60.4(2) ? ? ? yes
O(3) K O(5) 119.6(2) ? ? ? yes
O(3) K O(6) 95.8(1) ? ? ? yes
O(3) K O(6) 84.2(1) ? ? ? yes
O(4) K O(4) 180.0000 ? ? ? yes
O(4) K O(5) 61.4(2) ? ? ? yes
O(4) K O(5) 118.6(2) ? ? ? yes
O(4) K O(6) 73.3(1) ? ? ? yes
O(4) K O(6) 106.7(1) ? ? ? yes
O(4) K O(5) 118.6(2) ? ? ? yes
O(4) K O(5) 61.4(2) ? ? ? yes
O(4) K O(6) 106.7(1) ? ? ? yes
O(4) K O(6) 73.3(1) ? ? ? yes
O(5) K O(5) 180.0000 ? ? ? yes
O(5) K O(6) 87.8(1) ? ? ? yes
O(5) K O(6) 92.2(1) ? ? ? yes
O(5) K O(6) 92.2(1) ? ? ? yes
O(5) K O(6) 87.8(1) ? ? ? yes
O(6) K O(6) 180.0000 ? ? ? yes
Mn O(1) C(2) 125.0(4) ? ? ? yes
Mn O(2) C(11) 127.0(4) ? ? ? yes
K O(3) C(16) 106.8(4) ? ? ? yes
K O(3) C(21) 109.1(5) ? ? ? yes
C(16) O(3) C(21) 111.3(7) ? ? ? yes
K O(4) C(17) 124.2(5) ? ? ? yes
K O(4) C(18) 118.0(4) ? ? ? yes
C(17) O(4) C(18) 115.2(6) ? ? ? yes
K O(5) C(19) 106.8(4) ? ? ? yes
K O(5) C(20) 111.9(4) ? ? ? yes
C(19) O(5) C(20) 114.0(8) ? ? ? yes
K O(6) C(22) 127.8(4) ? ? ? yes
Mn N(1) C(4) 123.8(5) ? ? ? yes
Mn N(1) C(6) 111.1(7) ? ? ? yes
C(4) N(1) C(6) 123.7(7) ? ? ? yes
Mn N(2) C(7) 108.6(7) ? ? ? yes
Mn N(2) C(9) 127.1(7) ? ? ? yes
C(7) N(2) C(9) 123.9(8) ? ? ? yes
Mn N(3) C(13) 152.0(3) ? ? ? yes
Mn N(4) C(14) 154.8(3) ? ? ? yes
O(1) C(2) C(1) 112.8(7) ? ? ? yes
O(1) C(2) C(3) 124.1(7) ? ? ? yes
C(1) C(2) C(3) 123.1(7) ? ? ? yes
C(2) C(3) C(4) 128.6(8) ? ? ? yes
N(1) C(4) C(3) 122.0(6) ? ? ? yes
N(1) C(4) C(5) 119(1) ? ? ? yes
C(3) C(4) C(5) 118(1) ? ? ? yes
N(1) C(6) C(7) 118.3(9) ? ? ? yes
N(2) C(7) C(6) 116.4(9) ? ? ? yes
N(2) C(9) C(8) 122(1) ? ? ? yes
N(2) C(9) C(10) 121.0(8) ? ? ? yes
C(8) C(9) C(10) 116(1) ? ? ? yes
C(9) C(10) C(11) 129.9(9) ? ? ? yes
O(2) C(11) C(10) 122.7(7) ? ? ? yes
O(2) C(11) C(12) 113.1(7) ? ? ? yes
C(10) C(11) C(12) 124.2(7) ? ? ? yes
Fe C(13) N(3) 176.8(3) ? ? ? yes
Fe C(14) N(4) 178.4(3) ? ? ? yes
Fe C(15) N(5) 177.7(3) ? ? ? yes
O(3) C(16) C(17) 109.1(6) ? ? ? yes
O(4) C(17) C(16) 107.6(6) ? ? ? yes
O(4) C(18) C(19) 108.2(5) ? ? ? yes
O(5) C(19) C(18) 110.6(7) ? ? ? yes
O(5) C(20) C(21) 107.1(8) ? ? ? yes
O(3) C(21) C(20) 105.6(8) ? ? ? yes
O(6) C(22) C(23) 107(1) ? ? ? yes
O(6) C(22) C(24) 113.3(8) ? ? ? yes
C(23) C(22) C(24) 99(1) ? ? ? yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe C(13) 1.947(3) ? ? yes
Fe C(13) 1.947(3) ? ? yes
Fe C(14) 1.954(3) ? ? yes
Fe C(14) 1.954(3) ? ? yes
Fe C(15) 1.955(3) ? ? yes
Fe C(15) 1.955(3) ? ? yes
Mn O(1) 1.888(3) ? ? yes
Mn O(2) 1.892(3) ? ? yes
Mn N(1) 1.944(4) ? ? yes
Mn N(2) 1.968(5) ? ? yes
Mn N(3) 2.331(3) ? ? yes
Mn N(4) 2.439(3) ? ? yes
K O(3) 2.877(4) ? ? yes
K O(3) 2.877(4) ? ? yes
K O(4) 2.672(3) ? ? yes
K O(4) 2.672(3) ? ? yes
K O(5) 2.792(4) ? ? yes
K O(5) 2.792(4) ? ? yes
K O(6) 2.794(4) ? ? yes
K O(6) 2.794(4) ? ? yes
O(1) C(2) 1.296(6) ? ? yes
O(2) C(11) 1.300(6) ? ? yes
O(3) C(16) 1.459(10) ? ? yes
O(3) C(21) 1.41(1) ? ? yes
O(4) C(17) 1.372(10) ? ? yes
O(4) C(18) 1.43(1) ? ? yes
O(5) C(19) 1.40(1) ? ? yes
O(5) C(20) 1.44(1) ? ? yes
O(6) C(22) 1.376(8) ? ? yes
N(1) C(4) 1.32(1) ? ? yes
N(1) C(6) 1.45(1) ? ? yes
N(2) C(7) 1.51(1) ? ? yes
N(2) C(9) 1.27(1) ? ? yes
N(3) C(13) 1.153(4) ? ? yes
N(4) C(14) 1.143(4) ? ? yes
N(5) C(15) 1.151(4) ? ? yes
C(1) C(2) 1.50(1) ? ? yes
C(2) C(3) 1.35(1) ? ? yes
C(3) C(4) 1.35(1) ? ? yes
C(4) C(5) 1.520(9) ? ? yes
C(6) C(7) 1.27(2) ? ? yes
C(8) C(9) 1.52(1) ? ? yes
C(9) C(10) 1.37(2) ? ? yes
C(10) C(11) 1.36(1) ? ? yes
C(11) C(12) 1.499(9) ? ? yes
C(16) C(17) 1.45(1) ? ? yes
C(18) C(19) 1.44(1) ? ? yes
C(20) C(21) 1.48(1) ? ? yes
C(22) C(23) 1.21(2) ? ? yes
C(22) C(24) 1.34(1) ? ? yes
