#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:41:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179389 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/86/4328694.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_4328694
loop_
_publ_author_name
'Tapas Senapati'
'Céline Pichon'
'Rodica Ababei'
'Corine Mathonière'
'Rodolphe Clérac'
_publ_contact_author
;
        Rodolphe Clerac
        Centre de Recherche Paul Pascal
    115 avenue du Dr Schweitzer
        33600 PESSAC
    FRANCE
;
_publ_contact_author_email       clerac@crpp-bordeaux.cnrs.fr
_publ_contact_author_fax         '(33)5 56 84 56 00'
_publ_contact_author_phone       '(33)5 56 84 56 50'
_publ_section_title
;
 Cyanido-Bridged Fe(III)-Mn(III) Heterobimetallic Materials Built From
 Mn(III) Schiff Base Complexes and Di- or Tri-Cyanido Fe(III) Precursors
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3796
_journal_page_last               3812
_journal_paper_doi               10.1021/ic2027708
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C32 H24 Fe Mn N8 O4'
_chemical_formula_weight         695.38
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.64(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.348(5)
_cell_length_b                   23.946(5)
_cell_length_c                   13.121(4)
_cell_measurement_reflns_used    31668
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      1.00
_cell_volume                     2906.1(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0217
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16618
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.988
_exptl_absorpt_correction_T_max  0.8579
_exptl_absorpt_correction_T_min  0.7559
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_description       block
_exptl_crystal_F_000             1420
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.412
_refine_diff_density_min         -2.073
_refine_diff_density_rms         0.470
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.848
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         8512
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.848
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1302
_refine_ls_wR_factor_ref         0.2013
_reflns_number_gt                6777
_reflns_number_total             8512
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic2027708_si_003.cif
_cod_data_source_block           compound_3
_cod_original_cell_volume        2906.1(18)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4328694
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Fe1 Fe -0.25470(3) -0.099002(14) -0.73832(3) 0.01037(12) Uani 1 1 d .
Mn1 Mn 0.25044(3) -0.089991(15) -0.73415(3) 0.01089(12) Uani 1 1 d .
O1 O -0.5426(2) -0.19332(8) -0.98716(16) 0.0270(4) Uani 1 1 d .
O2 O -0.45929(19) -0.09790(7) -1.07924(15) 0.0226(4) Uani 1 1 d .
O3 O 0.16574(16) -0.03216(6) -0.83957(13) 0.0156(3) Uani 1 1 d .
O4 O 0.23819(17) -0.13923(7) -0.85102(13) 0.0154(3) Uani 1 1 d .
N1 N -0.29497(19) -0.17421(8) -0.69680(16) 0.0141(4) Uani 1 1 d .
N2 N -0.37965(19) -0.12277(8) -0.88804(15) 0.0133(3) Uani 1 1 d .
N3 N -0.24974(18) -0.02983(7) -0.81652(15) 0.0118(3) Uani 1 1 d .
N4 N -0.5178(2) -0.05921(9) -0.70241(17) 0.0188(4) Uani 1 1 d .
N5 N -0.0437(2) -0.06994(9) -0.48863(17) 0.0210(4) Uani 1 1 d .
N6 N 0.0319(2) -0.12484(8) -0.75140(17) 0.0180(4) Uani 1 1 d .
N7 N 0.25559(19) -0.04196(8) -0.60701(15) 0.0148(4) Uani 1 1 d .
N8 N 0.35308(19) -0.14979(8) -0.61848(16) 0.0140(4) Uani 1 1 d .
C1 C -0.2424(2) -0.19837(10) -0.5937(2) 0.0191(5) Uani 1 1 d .
H1 H -0.1705 -0.1801 -0.5316 0.023 Uiso 1 1 calc R
C2 C -0.2921(3) -0.24975(10) -0.5768(2) 0.0254(5) Uani 1 1 d .
H2 H -0.2528 -0.2657 -0.5045 0.031 Uiso 1 1 calc R
C3 C -0.3999(3) -0.27702(10) -0.6677(2) 0.0244(5) Uani 1 1 d .
H3 H -0.4348 -0.3113 -0.6577 0.029 Uiso 1 1 calc R
C4 C -0.4553(3) -0.25214(10) -0.7749(2) 0.0207(5) Uani 1 1 d .
H4 H -0.5288 -0.2694 -0.8376 0.025 Uiso 1 1 calc R
C5 C -0.3998(2) -0.20140(9) -0.7870(2) 0.0158(4) Uani 1 1 d .
C6 C -0.4503(2) -0.17273(9) -0.90013(19) 0.0161(4) Uani 1 1 d .
C7 C -0.3967(2) -0.08779(9) -0.97788(19) 0.0140(4) Uani 1 1 d .
C8 C -0.3219(2) -0.03318(9) -0.93100(18) 0.0132(4) Uani 1 1 d .
C9 C -0.3263(2) 0.01058(9) -1.00181(19) 0.0166(4) Uani 1 1 d .
H9 H -0.3771 0.0072 -1.0806 0.020 Uiso 1 1 calc R
C10 C -0.2531(2) 0.05943(10) -0.9522(2) 0.0201(5) Uani 1 1 d .
H10 H -0.2536 0.0895 -0.9972 0.024 Uiso 1 1 calc R
C11 C -0.1794(2) 0.06266(10) -0.8349(2) 0.0189(4) Uani 1 1 d .
H11 H -0.1304 0.0952 -0.8003 0.023 Uiso 1 1 calc R
C12 C -0.1784(2) 0.01740(9) -0.76851(19) 0.0159(4) Uani 1 1 d .
H12 H -0.1276 0.0198 -0.6895 0.019 Uiso 1 1 calc R
C13 C -0.4159(2) -0.07102(9) -0.71191(18) 0.0136(4) Uani 1 1 d .
C14 C -0.1228(2) -0.07836(9) -0.58220(19) 0.0145(4) Uani 1 1 d .
C15 C -0.0767(2) -0.11960(9) -0.74741(18) 0.0130(4) Uani 1 1 d .
C16 C 0.1633(2) 0.02203(9) -0.82192(19) 0.0143(4) Uani 1 1 d .
C17 C 0.1157(2) 0.05844(10) -0.9172(2) 0.0179(4) Uani 1 1 d .
H17 H 0.0882 0.0438 -0.9896 0.021 Uiso 1 1 calc R
C18 C 0.1098(3) 0.11550(10) -0.9034(2) 0.0225(5) Uani 1 1 d .
H18 H 0.0808 0.1389 -0.9664 0.027 Uiso 1 1 calc R
C19 C 0.1470(3) 0.13847(10) -0.7958(2) 0.0252(5) Uani 1 1 d .
H19 H 0.1430 0.1769 -0.7871 0.030 Uiso 1 1 calc R
C20 C 0.1898(2) 0.10364(10) -0.7026(2) 0.0211(5) Uani 1 1 d .
H20 H 0.2113 0.1188 -0.6316 0.025 Uiso 1 1 calc R
C21 C 0.2015(2) 0.04557(9) -0.71290(19) 0.0159(4) Uani 1 1 d .
C22 C 0.2362(2) 0.01154(10) -0.61411(19) 0.0164(4) Uani 1 1 d .
H22 H 0.2457 0.0298 -0.5485 0.020 Uiso 1 1 calc R
C23 C 0.2679(2) -0.07020(10) -0.50322(19) 0.0190(5) Uani 1 1 d .
H23A H 0.1928 -0.0984 -0.5248 0.023 Uiso 1 1 calc R
H23B H 0.2514 -0.0431 -0.4554 0.023 Uiso 1 1 calc R
C24 C 0.4142(3) -0.09791(12) -0.4341(2) 0.0248(5) Uani 1 1 d .
H24A H 0.4079 -0.1214 -0.3763 0.030 Uiso 1 1 calc R
H24B H 0.4854 -0.0691 -0.3952 0.030 Uiso 1 1 calc R
C25 C 0.4670(2) -0.13352(10) -0.50523(19) 0.0184(4) Uani 1 1 d .
H25A H 0.5409 -0.1128 -0.5155 0.022 Uiso 1 1 calc R
H25B H 0.5116 -0.1671 -0.4627 0.022 Uiso 1 1 calc R
C26 C 0.3283(2) -0.20208(9) -0.64243(19) 0.0162(4) Uani 1 1 d .
H26 H 0.3680 -0.2271 -0.5820 0.019 Uiso 1 1 calc R
C27 C 0.2446(2) -0.22515(10) -0.75420(19) 0.0153(4) Uani 1 1 d .
C28 C 0.2168(3) -0.28332(10) -0.7635(2) 0.0214(5) Uani 1 1 d .
H28 H 0.2401 -0.3042 -0.6978 0.026 Uiso 1 1 calc R
C29 C 0.1559(3) -0.30949(10) -0.8681(2) 0.0238(5) Uani 1 1 d .
H29 H 0.1344 -0.3474 -0.8735 0.029 Uiso 1 1 calc R
C30 C 0.1269(3) -0.27832(10) -0.9659(2) 0.0215(5) Uani 1 1 d .
H30 H 0.0885 -0.2959 -1.0366 0.026 Uiso 1 1 calc R
C31 C 0.1545(2) -0.22136(10) -0.9591(2) 0.0181(4) Uani 1 1 d .
H31 H 0.1353 -0.2015 -1.0253 0.022 Uiso 1 1 calc R
C32 C 0.2110(2) -0.19337(9) -0.85420(19) 0.0132(4) Uani 1 1 d .
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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'
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_3
N2 Fe1 N3 82.92(8) .
N2 Fe1 C15 94.84(9) .
N3 Fe1 C15 86.27(8) .
N2 Fe1 C13 92.67(9) .
N3 Fe1 C13 91.59(8) .
C15 Fe1 C13 171.87(9) .
N2 Fe1 C14 177.14(9) .
N3 Fe1 C14 99.52(9) .
C15 Fe1 C14 83.87(9) .
C13 Fe1 C14 88.75(9) .
N2 Fe1 N1 83.21(8) .
N3 Fe1 N1 166.08(8) .
C15 Fe1 N1 96.15(8) .
C13 Fe1 N1 87.80(8) .
C14 Fe1 N1 94.37(9) .
O3 Mn1 O4 91.32(7) .
O3 Mn1 N8 176.49(7) .
O4 Mn1 N8 89.35(8) .
O3 Mn1 N7 91.11(8) .
O4 Mn1 N7 175.81(7) .
N8 Mn1 N7 88.42(8) .
O3 Mn1 N6 94.63(8) .
O4 Mn1 N6 89.35(7) .
N8 Mn1 N6 88.82(8) .
N7 Mn1 N6 87.06(8) .
O3 Mn1 N4 90.08(8) 1_655
O4 Mn1 N4 91.79(7) 1_655
N8 Mn1 N4 86.45(8) 1_655
N7 Mn1 N4 91.61(8) 1_655
N6 Mn1 N4 175.12(7) 1_655
C16 O3 Mn1 129.51(15) .
C32 O4 Mn1 124.87(14) .
C5 N1 C1 118.4(2) .
C5 N1 Fe1 112.35(15) .
C1 N1 Fe1 129.02(16) .
C6 N2 C7 124.59(19) .
C6 N2 Fe1 117.56(15) .
C7 N2 Fe1 117.83(14) .
C12 N3 C8 119.12(19) .
C12 N3 Fe1 127.13(15) .
C8 N3 Fe1 113.67(14) .
C13 N4 Mn1 144.24(18) 1_455
C15 N6 Mn1 151.70(18) .
C22 N7 C23 117.9(2) .
C22 N7 Mn1 124.20(16) .
C23 N7 Mn1 117.66(15) .
C26 N8 C25 118.95(19) .
C26 N8 Mn1 121.89(16) .
C25 N8 Mn1 119.04(15) .
C2 C1 N1 122.1(2) .
C2 C1 H1 119.0 .
N1 C1 H1 119.0 .
C1 C2 C3 119.7(2) .
C1 C2 H2 120.2 .
C3 C2 H2 120.2 .
C4 C3 C2 118.6(2) .
C4 C3 H3 120.7 .
C2 C3 H3 120.7 .
C5 C4 C3 119.2(2) .
C5 C4 H4 120.4 .
C3 C4 H4 120.4 .
N1 C5 C4 122.0(2) .
N1 C5 C6 115.46(19) .
C4 C5 C6 122.5(2) .
O1 C6 N2 127.9(2) .
O1 C6 C5 121.4(2) .
N2 C6 C5 110.67(19) .
O2 C7 N2 127.6(2) .
O2 C7 C8 123.1(2) .
N2 C7 C8 109.30(18) .
N3 C8 C9 122.5(2) .
N3 C8 C7 115.75(19) .
C9 C8 C7 121.8(2) .
C8 C9 C10 118.4(2) .
C8 C9 H9 120.8 .
C10 C9 H9 120.8 .
C9 C10 C11 118.9(2) .
C9 C10 H10 120.5 .
C11 C10 H10 120.5 .
C12 C11 C10 120.1(2) .
C12 C11 H11 120.0 .
C10 C11 H11 120.0 .
N3 C12 C11 121.0(2) .
N3 C12 H12 119.5 .
C11 C12 H12 119.5 .
N4 C13 Fe1 173.2(2) .
N5 C14 Fe1 175.4(2) .
N6 C15 Fe1 171.62(19) .
O3 C16 C17 118.4(2) .
O3 C16 C21 123.3(2) .
C17 C16 C21 118.3(2) .
C18 C17 C16 120.7(2) .
C18 C17 H17 119.7 .
C16 C17 H17 119.7 .
C17 C18 C19 120.8(2) .
C17 C18 H18 119.6 .
C19 C18 H18 119.6 .
C18 C19 C20 119.4(2) .
C18 C19 H19 120.3 .
C20 C19 H19 120.3 .
C21 C20 C19 121.3(2) .
C21 C20 H20 119.3 .
C19 C20 H20 119.3 .
C22 C21 C20 118.2(2) .
C22 C21 C16 121.9(2) .
C20 C21 C16 119.5(2) .
N7 C22 C21 126.6(2) .
N7 C22 H22 116.7 .
C21 C22 H22 116.7 .
N7 C23 C24 113.65(19) .
N7 C23 H23A 108.8 .
C24 C23 H23A 108.8 .
N7 C23 H23B 108.8 .
C24 C23 H23B 108.8 .
H23A C23 H23B 107.7 .
C23 C24 C25 114.17(19) .
C23 C24 H24A 108.7 .
C25 C24 H24A 108.7 .
C23 C24 H24B 108.7 .
C25 C24 H24B 108.7 .
H24A C24 H24B 107.6 .
N8 C25 C24 114.68(18) .
N8 C25 H25A 108.6 .
C24 C25 H25A 108.6 .
N8 C25 H25B 108.6 .
C24 C25 H25B 108.6 .
H25A C25 H25B 107.6 .
N8 C26 C27 125.8(2) .
N8 C26 H26 117.1 .
C27 C26 H26 117.1 .
C26 C27 C28 118.2(2) .
C26 C27 C32 121.5(2) .
C28 C27 C32 119.5(2) .
C29 C28 C27 121.2(2) .
C29 C28 H28 119.4 .
C27 C28 H28 119.4 .
C28 C29 C30 119.1(2) .
C28 C29 H29 120.4 .
C30 C29 H29 120.4 .
C29 C30 C31 120.9(2) .
C29 C30 H30 119.6 .
C31 C30 H30 119.6 .
C32 C31 C30 121.1(2) .
C32 C31 H31 119.5 .
C30 C31 H31 119.5 .
O4 C32 C31 119.2(2) .
O4 C32 C27 122.4(2) .
C31 C32 C27 118.2(2) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N2 1.891(2) .
Fe1 N3 1.9612(19) .
Fe1 C15 1.961(2) .
Fe1 C13 1.967(2) .
Fe1 C14 1.948(2) .
Fe1 N1 1.9792(19) .
Mn1 O3 1.8740(16) .
Mn1 O4 1.8930(17) .
Mn1 N8 2.0092(19) .
Mn1 N7 2.0072(19) .
Mn1 N6 2.324(2) .
Mn1 N4 2.360(2) 1_655
O1 C6 1.217(3) .
O2 C7 1.214(3) .
O3 C16 1.320(3) .
O4 C32 1.323(3) .
N1 C5 1.360(3) .
N1 C1 1.342(3) .
N2 C6 1.373(3) .
N2 C7 1.391(3) .
N3 C12 1.343(3) .
N3 C8 1.347(3) .
N4 C13 1.151(3) .
N4 Mn1 2.360(2) 1_455
N5 C14 1.147(3) .
N6 C15 1.155(3) .
N7 C22 1.294(3) .
N7 C23 1.474(3) .
N8 C26 1.288(3) .
N8 C25 1.476(3) .
C1 C2 1.389(3) .
C1 H1 0.9300 .
C2 C3 1.379(4) .
C2 H2 0.9300 .
C3 C4 1.392(4) .
C3 H3 0.9300 .
C4 C5 1.384(3) .
C4 H4 0.9300 .
C5 C6 1.501(3) .
C7 C8 1.503(3) .
C8 C9 1.388(3) .
C9 C10 1.387(3) .
C9 H9 0.9300 .
C10 C11 1.380(3) .
C10 H10 0.9300 .
C11 C12 1.387(3) .
C11 H11 0.9300 .
C12 H12 0.9300 .
C16 C17 1.419(3) .
C16 C21 1.419(3) .
C17 C18 1.383(3) .
C17 H17 0.9300 .
C18 C19 1.399(4) .
C18 H18 0.9300 .
C19 C20 1.379(4) .
C19 H19 0.9300 .
C20 C21 1.407(3) .
C20 H20 0.9300 .
C21 C22 1.434(3) .
C22 H22 0.9300 .
C23 C24 1.524(3) .
C23 H23A 0.9700 .
C23 H23B 0.9700 .
C24 C25 1.535(3) .
C24 H24A 0.9700 .
C24 H24B 0.9700 .
C25 H25A 0.9700 .
C25 H25B 0.9700 .
C26 C27 1.438(3) .
C26 H26 0.9300 .
C27 C28 1.417(3) .
C27 C32 1.419(3) .
C28 C29 1.377(4) .
C28 H28 0.9300 .
C29 C30 1.396(4) .
C29 H29 0.9300 .
C30 C31 1.388(3) .
C30 H30 0.9300 .
C31 C32 1.402(3) .
C31 H31 0.9300 .
