#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:41:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179389 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/86/4328695.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_4328695
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_moiety         'C35 H30 Fe Mn N8 O4'
_chemical_formula_sum            'C35 H30 Fe Mn N8 O4'
_chemical_formula_weight         737.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.467(5)
_cell_length_b                   12.780(5)
_cell_length_c                   24.077(5)
_cell_measurement_temperature    150(2)
_cell_volume                     3221(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1710
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            7303
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.896
_exptl_absorpt_correction_T_max  0.8553
_exptl_absorpt_correction_T_min  0.8069
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       block
_exptl_crystal_F_000             1516
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.336
_refine_diff_density_min         -1.026
_refine_diff_density_rms         0.272
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         7303
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1661
_refine_ls_R_factor_gt           0.0670
_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)+(0.1227P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1450
_refine_ls_wR_factor_ref         0.2269
_reflns_number_gt                4167
_reflns_number_total             7303
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2027708_si_004.cif
_cod_data_source_block           Compound_4
_cod_database_code               4328695
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -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
Mn1 Mn 0.13417(10) -0.01102(9) 0.63809(5) 0.0200(3) Uani 1 1 d .
Fe1 Fe 0.63664(10) -0.03415(9) 0.65593(5) 0.0228(3) Uani 1 1 d .
O1 O 0.0888(5) -0.0342(4) 0.7133(2) 0.0214(12) Uani 1 1 d .
O2 O 0.1660(5) -0.1539(4) 0.6238(2) 0.0269(14) Uani 1 1 d .
O3 O 0.6557(7) -0.2008(5) 0.7964(3) 0.0538(19) Uani 1 1 d .
O4 O 0.7297(7) 0.0097(7) 0.8157(3) 0.056(2) Uani 1 1 d .
N1 N 0.0987(6) 0.1427(5) 0.6437(3) 0.0240(16) Uani 1 1 d .
N2 N 0.2019(6) 0.0339(6) 0.5642(3) 0.0238(16) Uani 1 1 d .
N3 N -0.0793(6) -0.0424(6) 0.6221(3) 0.0273(17) Uani 1 1 d .
N4 N 0.3454(6) 0.0002(5) 0.6689(3) 0.0242(15) Uani 1 1 d .
N5 N 0.5894(7) 0.0243(6) 0.5328(3) 0.0339(19) Uani 1 1 d .
N6 N 0.6153(6) -0.1856(5) 0.6498(3) 0.0297(18) Uani 1 1 d .
N7 N 0.6666(6) -0.0654(6) 0.7318(3) 0.0295(18) Uani 1 1 d .
N8 N 0.6665(5) 0.1107(6) 0.6812(3) 0.0248(17) Uani 1 1 d .
C1 C 0.0805(6) 0.0353(6) 0.7534(3) 0.0180(17) Uani 1 1 d .
C2 C 0.0708(7) -0.0012(7) 0.8082(3) 0.0273(19) Uani 1 1 d .
H2 H 0.0716 -0.0727 0.8153 0.033 Uiso 1 1 calc R
C3 C 0.0600(7) 0.0695(7) 0.8518(3) 0.029(2) Uani 1 1 d .
H3 H 0.0544 0.0446 0.8880 0.035 Uiso 1 1 calc R
C4 C 0.0576(7) 0.1792(7) 0.8421(4) 0.029(2) Uani 1 1 d .
H4 H 0.0518 0.2256 0.8717 0.035 Uiso 1 1 calc R
C5 C 0.0637(8) 0.2160(7) 0.7886(3) 0.0259(19) Uani 1 1 d .
H5 H 0.0600 0.2877 0.7820 0.031 Uiso 1 1 calc R
C6 C 0.0756(7) 0.1466(6) 0.7438(3) 0.0218(18) Uani 1 1 d .
C7 C 0.0822(7) 0.1920(7) 0.6891(3) 0.0227(19) Uani 1 1 d .
H7 H 0.0736 0.2643 0.6868 0.027 Uiso 1 1 calc R
C8 C 0.0932(8) 0.1981(7) 0.5878(4) 0.028(2) Uani 1 1 d .
C9 C 0.1058(9) 0.3178(7) 0.5934(4) 0.041(3) Uani 1 1 d .
H9A H 0.0305 0.3454 0.6108 0.061 Uiso 1 1 calc R
H9B H 0.1157 0.3484 0.5573 0.061 Uiso 1 1 calc R
H9C H 0.1792 0.3340 0.6157 0.061 Uiso 1 1 calc R
C10 C -0.0380(8) 0.1708(8) 0.5613(4) 0.037(2) Uani 1 1 d .
H10A H -0.0383 0.0986 0.5502 0.055 Uiso 1 1 calc R
H10B H -0.0520 0.2143 0.5294 0.055 Uiso 1 1 calc R
H10C H -0.1047 0.1825 0.5879 0.055 Uiso 1 1 calc R
C11 C 0.2062(8) 0.1523(7) 0.5527(4) 0.029(2) Uani 1 1 d .
C12 C 0.3368(8) 0.1966(7) 0.5741(4) 0.033(2) Uani 1 1 d .
H12A H 0.3425 0.1869 0.6136 0.050 Uiso 1 1 calc R
H12B H 0.3422 0.2699 0.5656 0.050 Uiso 1 1 calc R
H12C H 0.4057 0.1602 0.5563 0.050 Uiso 1 1 calc R
C13 C 0.1907(8) 0.1762(8) 0.4906(4) 0.034(2) Uani 1 1 d .
H13A H 0.2672 0.1564 0.4712 0.051 Uiso 1 1 calc R
H13B H 0.1757 0.2497 0.4856 0.051 Uiso 1 1 calc R
H13C H 0.1197 0.1374 0.4761 0.051 Uiso 1 1 calc R
C14 C 0.2711(7) -0.0284(8) 0.5333(4) 0.031(2) Uani 1 1 d .
H14 H 0.3189 0.0033 0.5055 0.037 Uiso 1 1 calc R
C15 C 0.2821(8) -0.1405(7) 0.5375(4) 0.029(2) Uani 1 1 d .
C16 C 0.3529(11) -0.1929(8) 0.4960(4) 0.044(3) Uani 1 1 d .
H16 H 0.3967 -0.1544 0.4693 0.053 Uiso 1 1 calc R
C17 C 0.3573(11) -0.2978(8) 0.4948(4) 0.043(2) Uani 1 1 d .
H17 H 0.4030 -0.3312 0.4669 0.051 Uiso 1 1 calc R
C18 C 0.2956(9) -0.3562(8) 0.5341(4) 0.036(2) Uani 1 1 d .
H18 H 0.2962 -0.4288 0.5318 0.043 Uiso 1 1 calc R
C19 C 0.2332(7) -0.3079(7) 0.5766(4) 0.029(2) Uani 1 1 d .
H19 H 0.1950 -0.3487 0.6040 0.035 Uiso 1 1 calc R
C20 C 0.2246(7) -0.1976(7) 0.5805(4) 0.0247(19) Uani 1 1 d .
C21 C 0.4545(7) -0.0152(6) 0.6645(3) 0.0219(18) Uani 1 1 d .
C22 C 0.5928(8) -0.2427(8) 0.6037(5) 0.040(3) Uani 1 1 d .
H22 H 0.5889 -0.2095 0.5694 0.049 Uiso 1 1 calc R
C23 C 0.5751(9) -0.3515(8) 0.6067(5) 0.045(3) Uani 1 1 d .
H23 H 0.5602 -0.3899 0.5746 0.054 Uiso 1 1 calc R
C24 C 0.5799(8) -0.4017(8) 0.6581(5) 0.050(3) Uani 1 1 d .
H24 H 0.5670 -0.4735 0.6607 0.060 Uiso 1 1 calc R
C25 C 0.6038(8) -0.3438(8) 0.7041(5) 0.044(3) Uani 1 1 d .
H25 H 0.6089 -0.3769 0.7384 0.053 Uiso 1 1 calc R
C26 C 0.6215(8) -0.2319(7) 0.7010(4) 0.040(3) Uani 1 1 d .
C27 C 0.6507(8) -0.1667(7) 0.7488(4) 0.034(2) Uani 1 1 d .
C28 C 0.7016(8) 0.0158(8) 0.7662(4) 0.036(2) Uani 1 1 d .
C29 C 0.6986(8) 0.1188(8) 0.7348(4) 0.031(2) Uani 1 1 d .
C30 C 0.7220(8) 0.2136(9) 0.7597(4) 0.041(3) Uani 1 1 d .
H30 H 0.7449 0.2168 0.7970 0.050 Uiso 1 1 calc R
C31 C 0.7113(9) 0.3026(9) 0.7291(4) 0.044(3) Uani 1 1 d .
H31 H 0.7263 0.3674 0.7454 0.053 Uiso 1 1 calc R
C32 C 0.6782(9) 0.2960(8) 0.6740(4) 0.040(2) Uani 1 1 d .
H32 H 0.6710 0.3559 0.6523 0.048 Uiso 1 1 calc R
C33 C 0.6561(7) 0.1997(7) 0.6520(4) 0.032(2) Uani 1 1 d .
H33 H 0.6327 0.1953 0.6148 0.039 Uiso 1 1 calc R
C34 C 0.6078(6) 0.0001(7) 0.5777(4) 0.0256(19) Uani 1 1 d .
C35 C 0.8145(7) -0.0431(7) 0.6343(4) 0.0245(18) 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'
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'
Mn Mn 0.3368 0.7283 '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
O2 Mn1 O1 93.8(2) .
O2 Mn1 N2 93.0(3) .
O1 Mn1 N2 169.7(3) .
O2 Mn1 N1 173.3(3) .
O1 Mn1 N1 92.5(3) .
N2 Mn1 N1 81.0(3) .
O2 Mn1 N3 88.4(3) .
O1 Mn1 N3 83.6(2) .
N2 Mn1 N3 104.2(3) .
N1 Mn1 N3 90.1(3) .
O2 Mn1 N4 87.2(2) .
O1 Mn1 N4 86.7(2) .
N2 Mn1 N4 86.0(2) .
N1 Mn1 N4 95.4(3) .
N3 Mn1 N4 169.1(2) .
N7 Fe1 C21 94.9(3) .
N7 Fe1 C35 95.0(3) .
C21 Fe1 C35 169.9(3) .
N7 Fe1 N6 83.3(3) .
C21 Fe1 N6 91.1(3) .
C35 Fe1 N6 91.8(3) .
N7 Fe1 C34 179.0(3) .
C21 Fe1 C34 85.6(3) .
C35 Fe1 C34 84.4(3) .
N6 Fe1 C34 97.6(3) .
N7 Fe1 N8 82.8(3) .
C21 Fe1 N8 90.3(3) .
C35 Fe1 N8 89.2(3) .
N6 Fe1 N8 166.0(3) .
C34 Fe1 N8 96.4(3) .
C1 O1 Mn1 127.7(5) .
C20 O2 Mn1 129.0(5) .
C7 N1 C8 121.6(7) .
C7 N1 Mn1 124.6(6) .
C8 N1 Mn1 113.8(5) .
C14 N2 C11 118.7(7) .
C14 N2 Mn1 121.8(6) .
C11 N2 Mn1 116.9(5) .
C35 N3 Mn1 153.8(7) 1_455
C21 N4 Mn1 152.8(6) .
C22 N6 C26 121.1(8) .
C22 N6 Fe1 128.1(6) .
C26 N6 Fe1 110.8(7) .
C27 N7 C28 124.5(8) .
C27 N7 Fe1 117.8(6) .
C28 N7 Fe1 117.7(6) .
C29 N8 C33 117.4(8) .
C29 N8 Fe1 114.2(6) .
C33 N8 Fe1 128.4(6) .
O1 C1 C2 118.0(7) .
O1 C1 C6 123.4(7) .
C2 C1 C6 118.5(8) .
C3 C2 C1 120.0(8) .
C2 C3 C4 121.2(8) .
C5 C4 C3 119.5(8) .
C4 C5 C6 120.6(8) .
C5 C6 C7 116.9(8) .
C5 C6 C1 120.2(8) .
C7 C6 C1 122.9(7) .
N1 C7 C6 126.3(8) .
N1 C8 C9 112.4(7) .
N1 C8 C10 106.9(7) .
C9 C8 C10 109.6(7) .
N1 C8 C11 105.9(6) .
C9 C8 C11 110.7(7) .
C10 C8 C11 111.2(7) .
C13 C11 N2 111.6(7) .
C13 C11 C8 111.8(7) .
N2 C11 C8 104.4(7) .
C13 C11 C12 109.9(7) .
N2 C11 C12 108.8(7) .
C8 C11 C12 110.2(7) .
N2 C14 C15 127.6(8) .
C20 C15 C16 120.0(9) .
C20 C15 C14 122.3(8) .
C16 C15 C14 117.6(8) .
C17 C16 C15 120.5(9) .
C16 C17 C18 121.0(9) .
C19 C18 C17 120.0(9) .
C18 C19 C20 122.1(9) .
O2 C20 C15 123.9(8) .
O2 C20 C19 119.9(8) .
C15 C20 C19 116.3(8) .
N4 C21 Fe1 177.3(7) .
N6 C22 C23 121.0(10) .
C24 C23 C22 119.8(11) .
C25 C24 C23 118.7(10) .
C24 C25 C26 121.5(10) .
N6 C26 C25 117.9(10) .
N6 C26 C27 118.4(8) .
C25 C26 C27 123.7(9) .
O3 C27 N7 127.5(9) .
O3 C27 C26 123.0(9) .
N7 C27 C26 109.4(8) .
O4 C28 N7 126.7(10) .
O4 C28 C29 122.8(9) .
N7 C28 C29 110.5(8) .
N8 C29 C30 122.2(9) .
N8 C29 C28 114.7(8) .
C30 C29 C28 123.0(9) .
C31 C30 C29 119.2(9) .
C30 C31 C32 119.5(10) .
C33 C32 C31 118.3(10) .
N8 C33 C32 123.4(9) .
N5 C34 Fe1 177.0(8) .
N3 C35 Fe1 176.1(9) 1_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O2 1.888(6) .
Mn1 O1 1.896(5) .
Mn1 N2 2.000(7) .
Mn1 N1 2.003(7) .
Mn1 N3 2.302(7) .
Mn1 N4 2.337(6) .
Fe1 N7 1.897(7) .
Fe1 C21 1.933(7) .
Fe1 C35 1.937(8) .
Fe1 N6 1.954(7) .
Fe1 C34 1.958(9) .
Fe1 N8 1.974(7) .
O1 C1 1.315(9) .
O2 C20 1.332(10) .
O3 C27 1.228(11) .
O4 C28 1.232(11) .
N1 C7 1.275(10) .
N1 C8 1.522(10) .
N2 C14 1.308(11) .
N2 C11 1.540(11) .
N3 C35 1.150(9) 1_455
N4 C21 1.164(9) .
N5 C34 1.139(10) .
N6 C22 1.350(12) .
N6 C26 1.368(11) .
N7 C27 1.367(11) .
N7 C28 1.376(12) .
N8 C29 1.338(11) .
N8 C33 1.341(11) .
C1 C2 1.403(11) .
C1 C6 1.442(11) .
C2 C3 1.389(12) .
C3 C4 1.420(12) .
C4 C5 1.373(12) .
C5 C6 1.403(11) .
C6 C7 1.440(11) .
C8 C9 1.541(13) .
C8 C10 1.554(12) .
C8 C11 1.567(12) .
C11 C13 1.534(12) .
C11 C12 1.567(12) .
C14 C15 1.440(13) .
C15 C20 1.402(12) .
C15 C16 1.413(13) .
C16 C17 1.341(13) .
C17 C18 1.367(14) .
C18 C19 1.363(13) .
C19 C20 1.415(12) .
C22 C23 1.405(14) .
C23 C24 1.394(15) .
C24 C25 1.356(15) .
C25 C26 1.444(14) .
C26 C27 1.453(14) .
C28 C29 1.518(13) .
C29 C30 1.372(13) .
C30 C31 1.359(15) .
C31 C32 1.375(14) .
C32 C33 1.359(12) .
C35 N3 1.150(9) 1_655
