#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:26:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179141 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/02/4310252.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_4310252
loop_
_publ_author_name
'Zhong-Hai Ni'
'Hui-Zhong Kou'
'Li-Fang Zhang'
'Wei-Wei Ni'
'Yun-Bo Jiang'
'Ai-Li Cui'
'Joan Ribas'
'Osamu Sato'
_publ_section_title
;
mer-[Fe(pcq)(CN)3]-: A Novel Cyanide-Containing Building Block and Its
Application to Assembling Cyanide-Bridged Trinuclear FeIII2MnII Complexes
[pcq-= 8-(Pyridine-2-carboxamido)quinoline Anion]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9631
_journal_page_last               9633
_journal_paper_doi               10.1021/ic051385v
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C38 H32 Fe2 Mn N12 O6, 2(H2 O)'
_chemical_formula_sum            'C38 H36 Fe2 Mn N12 O8'
_chemical_formula_weight         955.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 113.302(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.125(16)
_cell_length_b                   14.483(10)
_cell_length_c                   15.061(12)
_cell_measurement_reflns_used    45
_cell_measurement_temperature    293(2)
_cell_volume                     4232(5)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku IP'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16791
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    1.035
_exptl_absorpt_correction_T_max  0.815
_exptl_absorpt_correction_T_min  0.783
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'SADABS (Bruker, 2000)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1956
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         4815
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0512P)²+5.0859P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1225
_reflns_number_gt                3685
_reflns_number_total             4815
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051385vsi20050815_120441_1.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4310252
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.13108(2) 0.77749(3) 0.14175(3) 0.02469(13) Uani 1 1 d . . .
Mn1 Mn 0.0000 0.51944(4) 0.2500 0.02923(18) Uani 1 2 d S . .
O1 O 0.29006(13) 0.90204(18) 0.1134(2) 0.0609(8) Uani 1 1 d . . .
O2 O -0.09480(12) 0.50688(16) 0.11864(19) 0.0457(6) Uani 1 1 d . . .
O3 O 0.04144(12) 0.40339(16) 0.1945(2) 0.0482(6) Uani 1 1 d . . .
O1W O 0.3281(2) 0.1560(2) 0.0316(3) 0.0784(11) Uani 1 1 d . . .
N3 N 0.04761(14) 0.62479(18) 0.1914(2) 0.0392(7) Uani 1 1 d . . .
N1 N 0.20136(19) 0.8159(2) 0.3623(2) 0.0588(9) Uani 1 1 d . . .
N2 N 0.05004(15) 0.72204(19) -0.0726(2) 0.0416(7) Uani 1 1 d . . .
N4 N 0.06704(12) 0.87904(15) 0.13158(17) 0.0255(5) Uani 1 1 d . . .
N5 N 0.18417(12) 0.87164(16) 0.11900(18) 0.0290(6) Uani 1 1 d . . .
N6 N 0.20687(13) 0.69928(17) 0.14302(19) 0.0317(6) Uani 1 1 d . . .
C3 C 0.07820(16) 0.6813(2) 0.1731(2) 0.0310(7) Uani 1 1 d . . .
C1 C 0.17554(17) 0.7985(2) 0.2815(2) 0.0354(7) Uani 1 1 d . . .
C2 C 0.08005(16) 0.7423(2) 0.0066(2) 0.0302(7) Uani 1 1 d . . .
C4 C 0.00517(16) 0.8766(2) 0.1340(2) 0.0315(7) Uani 1 1 d . . .
H4A H -0.0136 0.8198 0.1393 0.038 Uiso 1 1 calc R . .
C5 C -0.03304(18) 0.9569(2) 0.1289(2) 0.0388(8) Uani 1 1 d . . .
H5A H -0.0766 0.9528 0.1301 0.047 Uiso 1 1 calc R . .
C6 C -0.00676(19) 1.0402(2) 0.1222(2) 0.0421(8) Uani 1 1 d . . .
H6A H -0.0316 1.0936 0.1206 0.051 Uiso 1 1 calc R . .
C7 C 0.05884(18) 1.0463(2) 0.1176(2) 0.0360(7) Uani 1 1 d . . .
C8 C 0.0907(2) 1.1292(2) 0.1081(3) 0.0477(9) Uani 1 1 d . . .
H8A H 0.0693 1.1854 0.1072 0.057 Uiso 1 1 calc R . .
C9 C 0.1529(2) 1.1270(2) 0.1003(3) 0.0508(10) Uani 1 1 d . . .
H9A H 0.1730 1.1821 0.0934 0.061 Uiso 1 1 calc R . .
C10 C 0.18740(18) 1.0431(2) 0.1026(3) 0.0419(8) Uani 1 1 d . . .
H10A H 0.2295 1.0433 0.0965 0.050 Uiso 1 1 calc R . .
C11 C 0.09423(16) 0.96312(19) 0.1214(2) 0.0275(6) Uani 1 1 d . . .
C12 C 0.15874(16) 0.9614(2) 0.1137(2) 0.0306(7) Uani 1 1 d . . .
C13 C 0.24737(16) 0.8493(2) 0.1212(2) 0.0374(8) Uani 1 1 d . . .
C14 C 0.25805(16) 0.7475(2) 0.1318(2) 0.0366(7) Uani 1 1 d . . .
C15 C 0.3155(2) 0.7053(3) 0.1293(3) 0.0528(10) Uani 1 1 d . . .
H15A H 0.3508 0.7400 0.1238 0.063 Uiso 1 1 calc R . .
C16 C 0.3199(2) 0.6103(3) 0.1352(3) 0.0615(12) Uani 1 1 d . . .
H16A H 0.3582 0.5801 0.1333 0.074 Uiso 1 1 calc R . .
C17 C 0.2674(2) 0.5608(3) 0.1438(3) 0.0518(10) Uani 1 1 d . . .
H17A H 0.2693 0.4966 0.1463 0.062 Uiso 1 1 calc R . .
C18 C 0.21191(18) 0.6070(2) 0.1488(3) 0.0413(8) Uani 1 1 d . . .
H18A H 0.1769 0.5732 0.1563 0.050 Uiso 1 1 calc R . .
C19 C 0.0879(3) 0.4095(4) 0.1437(5) 0.117(3) Uani 1 1 d . . .
H19A H 0.0981 0.3486 0.1280 0.176 Uiso 1 1 calc R . .
H19B H 0.1299 0.4395 0.1845 0.176 Uiso 1 1 calc R . .
H19C H 0.0662 0.4446 0.0854 0.176 Uiso 1 1 calc R . .
H300 H 0.0083 0.3585 0.1640 0.083(15) Uiso 1 1 d R . .
H200 H -0.1287 0.5691 0.0841 0.098(16) Uiso 1 1 d R . .
H201 H -0.1205 0.4615 0.0965 0.11(2) Uiso 1 1 d R . .
H400 H 0.293(3) 0.160(3) -0.025(4) 0.087(17) Uiso 1 1 d . . .
H401 H 0.327(4) 0.207(5) 0.070(5) 0.14(3) Uiso 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'
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'
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
N5 Fe1 N6 82.93(12) . . ?
N5 Fe1 C2 97.01(12) . . ?
N6 Fe1 C2 88.36(12) . . ?
N5 Fe1 C3 176.81(12) . . ?
N6 Fe1 C3 97.38(13) . . ?
C2 Fe1 C3 86.17(13) . . ?
N5 Fe1 C1 90.92(12) . . ?
N6 Fe1 C1 92.12(13) . . ?
C2 Fe1 C1 172.05(13) . . ?
C3 Fe1 C1 85.90(13) . . ?
N5 Fe1 N4 83.38(12) . . ?
N6 Fe1 N4 166.25(10) . . ?
C2 Fe1 N4 91.99(11) . . ?
C3 Fe1 N4 96.36(13) . . ?
C1 Fe1 N4 89.43(12) . . ?
N3 Mn1 N3 91.94(15) . 2 ?
N3 Mn1 O2 91.15(11) . 2 ?
N3 Mn1 O2 95.45(11) 2 2 ?
N3 Mn1 O2 95.45(11) . . ?
N3 Mn1 O2 91.15(11) 2 . ?
O2 Mn1 O2 170.50(13) 2 . ?
N3 Mn1 O3 93.66(11) . . ?
N3 Mn1 O3 174.31(10) 2 . ?
O2 Mn1 O3 85.47(10) 2 . ?
O2 Mn1 O3 87.29(11) . . ?
N3 Mn1 O3 174.31(10) . 2 ?
N3 Mn1 O3 93.66(11) 2 2 ?
O2 Mn1 O3 87.29(11) 2 2 ?
O2 Mn1 O3 85.47(10) . 2 ?
O3 Mn1 O3 80.76(15) . 2 ?
Mn1 O2 H200 122.0 . . ?
Mn1 O2 H201 130.1 . . ?
H200 O2 H201 104.3 . . ?
C19 O3 Mn1 126.8(3) . . ?
C19 O3 H300 108.2 . . ?
Mn1 O3 H300 112.7 . . ?
H400 O1W H401 109(5) . . ?
C3 N3 Mn1 171.1(3) . . ?
C4 N4 C11 119.1(2) . . ?
C4 N4 Fe1 129.5(2) . . ?
C11 N4 Fe1 111.4(2) . . ?
C13 N5 C12 125.0(3) . . ?
C13 N5 Fe1 118.2(2) . . ?
C12 N5 Fe1 116.2(2) . . ?
C18 N6 C14 118.4(3) . . ?
C18 N6 Fe1 128.5(2) . . ?
C14 N6 Fe1 113.0(2) . . ?
N3 C3 Fe1 179.6(3) . . ?
N1 C1 Fe1 176.3(3) . . ?
N2 C2 Fe1 179.7(4) . . ?
N4 C4 C5 122.1(3) . . ?
N4 C4 H4A 119.0 . . ?
C5 C4 H4A 119.0 . . ?
C6 C5 C4 120.1(3) . . ?
C6 C5 H5A 119.9 . . ?
C4 C5 H5A 119.9 . . ?
C5 C6 C7 119.9(3) . . ?
C5 C6 H6A 120.1 . . ?
C7 C6 H6A 120.1 . . ?
C11 C7 C8 117.7(3) . . ?
C11 C7 C6 117.3(3) . . ?
C8 C7 C6 124.9(3) . . ?
C9 C8 C7 120.2(3) . . ?
C9 C8 H8A 119.9 . . ?
C7 C8 H8A 119.9 . . ?
C8 C9 C10 121.6(3) . . ?
C8 C9 H9A 119.2 . . ?
C10 C9 H9A 119.2 . . ?
C12 C10 C9 119.9(3) . . ?
C12 C10 H10A 120.1 . . ?
C9 C10 H10A 120.1 . . ?
N4 C11 C7 121.4(3) . . ?
N4 C11 C12 116.8(3) . . ?
C7 C11 C12 121.7(3) . . ?
C10 C12 N5 129.3(3) . . ?
C10 C12 C11 118.8(3) . . ?
N5 C12 C11 111.9(2) . . ?
O1 C13 N5 127.1(3) . . ?
O1 C13 C14 122.9(3) . . ?
N5 C13 C14 110.1(3) . . ?
N6 C14 C15 122.2(3) . . ?
N6 C14 C13 115.4(3) . . ?
C15 C14 C13 122.4(3) . . ?
C14 C15 C16 118.7(4) . . ?
C14 C15 H15A 120.7 . . ?
C16 C15 H15A 120.7 . . ?
C17 C16 C15 119.5(4) . . ?
C17 C16 H16A 120.2 . . ?
C15 C16 H16A 120.2 . . ?
C16 C17 C18 119.3(4) . . ?
C16 C17 H17A 120.3 . . ?
C18 C17 H17A 120.3 . . ?
N6 C18 C17 121.9(3) . . ?
N6 C18 H18A 119.1 . . ?
C17 C18 H18A 119.1 . . ?
O3 C19 H19A 109.5 . . ?
O3 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O3 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
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 N5 1.881(3) . ?
Fe1 N6 1.955(3) . ?
Fe1 C2 1.957(4) . ?
Fe1 C3 1.957(3) . ?
Fe1 C1 1.960(4) . ?
Fe1 N4 1.963(3) . ?
Mn1 N3 2.195(3) . ?
Mn1 N3 2.195(3) 2 ?
Mn1 O2 2.196(3) 2 ?
Mn1 O2 2.196(3) . ?
Mn1 O3 2.206(3) . ?
Mn1 O3 2.206(3) 2 ?
O1 C13 1.222(4) . ?
O2 H200 1.1405 . ?
O2 H201 0.8340 . ?
O3 C19 1.467(6) . ?
O3 H300 0.9331 . ?
O1W H400 0.88(5) . ?
O1W H401 0.95(7) . ?
N3 C3 1.142(4) . ?
N1 C1 1.148(4) . ?
N2 C2 1.146(4) . ?
N4 C4 1.322(4) . ?
N4 C11 1.381(4) . ?
N5 C13 1.362(4) . ?
N5 C12 1.397(4) . ?
N6 C18 1.341(4) . ?
N6 C14 1.353(4) . ?
C4 C5 1.400(4) . ?
C4 H4A 0.9300 . ?
C5 C6 1.348(5) . ?
C5 H5A 0.9300 . ?
C6 C7 1.417(5) . ?
C6 H6A 0.9300 . ?
C7 C11 1.407(4) . ?
C7 C8 1.411(5) . ?
C8 C9 1.365(6) . ?
C8 H8A 0.9300 . ?
C9 C10 1.409(5) . ?
C9 H9A 0.9300 . ?
C10 C12 1.370(4) . ?
C10 H10A 0.9300 . ?
C11 C12 1.413(4) . ?
C13 C14 1.490(5) . ?
C14 C15 1.374(5) . ?
C15 C16 1.379(6) . ?
C15 H15A 0.9300 . ?
C16 C17 1.368(6) . ?
C16 H16A 0.9300 . ?
C17 C18 1.378(5) . ?
C17 H17A 0.9300 . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
