#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/71/1517155.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_1517155
loop_
_publ_author_name
'Hongbo Zhou'
'Qian Zhang'
'Yuqi Yang'
'Yan Xu'
'Hu Zhou'
'Xiaoping Shen'
_publ_section_title
;
 Syntheses, crystal structures and magnetic properties of three
 cyano-bridged trinuclear clusters based on modified hexacyanometalates
 building blocksOriginal
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              97
_journal_page_last               103
_journal_volume                  402
_journal_year                    2013
_chemical_formula_moiety         'C48 H52 Fe2 N16 Ni, 4(C H4 O)'
_chemical_formula_sum            'C52 H68 Fe2 N16 Ni O4'
_chemical_formula_weight         1151.63
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 114.446(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.7448(16)
_cell_length_b                   19.343(3)
_cell_length_c                   14.2520(16)
_cell_measurement_reflns_used    2057
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      23.22
_cell_measurement_theta_min      2.28
_cell_volume                     2696.5(7)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Aepex CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0611
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20922
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.937
_exptl_absorpt_correction_T_max  0.8348
_exptl_absorpt_correction_T_min  0.7927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            'red brown'
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5296
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0613
_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)+(0.07P)²+1.88P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1389
_refine_ls_wR_factor_ref         0.1482
_reflns_number_gt                3862
_reflns_number_total             5296
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-402-97-103-3.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1517155
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
C1 C 0.5867(4) -0.0145(2) 0.7185(3) 0.0411(10) Uani 1 1 d .
H1 H 0.5610 -0.0139 0.6477 0.049 Uiso 1 1 calc R
C2 C 0.6544(4) -0.0716(2) 0.7762(3) 0.0435(10) Uani 1 1 d .
H2 H 0.6751 -0.1089 0.7442 0.052 Uiso 1 1 calc R
C3 C 0.6910(4) -0.0728(2) 0.8818(3) 0.0465(10) Uani 1 1 d .
H3 H 0.7372 -0.1109 0.9203 0.056 Uiso 1 1 calc R
C4 C 0.6589(4) -0.0169(2) 0.9312(3) 0.0416(9) Uani 1 1 d .
C5 C 0.6960(4) -0.0152(2) 1.0370(3) 0.0436(10) Uani 1 1 d .
H5 H 0.7399 -0.0529 1.0777 0.052 Uiso 1 1 calc R
C6 C 0.6673(4) 0.0432(2) 1.0817(3) 0.0414(10) Uani 1 1 d .
H6 H 0.6919 0.0445 1.1524 0.050 Uiso 1 1 calc R
C7 C 0.6018(4) 0.0994(2) 1.0205(3) 0.0395(9) Uani 1 1 d .
C8 C 0.5702(4) 0.1620(2) 1.0592(3) 0.0457(10) Uani 1 1 d .
H8 H 0.5963 0.1668 1.1297 0.055 Uiso 1 1 calc R
C9 C 0.5012(4) 0.2161(2) 0.9939(3) 0.0446(10) Uani 1 1 d .
H9 H 0.4815 0.2564 1.0206 0.053 Uiso 1 1 calc R
C10 C 0.4621(4) 0.2093(2) 0.8880(3) 0.0407(9) Uani 1 1 d .
H10 H 0.4151 0.2450 0.8440 0.049 Uiso 1 1 calc R
C11 C 0.5644(5) 0.0974(2) 0.9150(3) 0.0469(10) Uani 1 1 d .
C12 C 0.5937(4) 0.0391(2) 0.8703(3) 0.0411(9) Uani 1 1 d .
C13 C 0.2832(4) 0.0731(2) 0.6760(3) 0.0392(9) Uani 1 1 d .
C14 C 0.4306(4) 0.1057(2) 0.5646(3) 0.0419(9) Uani 1 1 d .
C15 C 0.3524(4) 0.2075(2) 0.6520(3) 0.0442(10) Uani 1 1 d .
C16 C 0.6275(4) 0.1757(2) 0.7272(3) 0.0370(9) Uani 1 1 d .
C17 C -0.1527(4) 0.1452(2) 0.4600(3) 0.0437(10) Uani 1 1 d .
C18 C -0.0482(5) 0.1632(2) 0.4180(3) 0.0490(11) Uani 1 1 d .
H18A H 0.0394 0.1706 0.4757 0.059 Uiso 1 1 calc R
H18B H -0.0748 0.2065 0.3806 0.059 Uiso 1 1 calc R
C19 C -0.0293(4) 0.1077(2) 0.3452(3) 0.0437(10) Uani 1 1 d .
H19 H -0.1172 0.0873 0.2998 0.052 Uiso 1 1 calc R
C20 C 0.1036(4) 0.0073(2) 0.3495(3) 0.0446(10) Uani 1 1 d .
H20A H 0.1640 0.0292 0.3232 0.053 Uiso 1 1 calc R
H20B H 0.0224 -0.0078 0.2910 0.053 Uiso 1 1 calc R
C21 C 0.1771(4) -0.0568(2) 0.4160(3) 0.0434(10) Uani 1 1 d .
H21A H 0.1901 -0.0924 0.3728 0.052 Uiso 1 1 calc R
H21B H 0.2659 -0.0437 0.4683 0.052 Uiso 1 1 calc R
C22 C -0.1626(4) 0.2146(2) 0.5224(3) 0.0457(10) Uani 1 1 d .
H22A H -0.2037 0.2514 0.4742 0.069 Uiso 1 1 calc R
H22B H -0.0725 0.2282 0.5698 0.069 Uiso 1 1 calc R
H22C H -0.2174 0.2050 0.5596 0.069 Uiso 1 1 calc R
C23 C -0.2951(4) 0.1295(2) 0.3854(3) 0.0507(12) Uani 1 1 d .
H23A H -0.3312 0.1681 0.3397 0.076 Uiso 1 1 calc R
H23B H -0.3509 0.1212 0.4222 0.076 Uiso 1 1 calc R
H23C H -0.2950 0.0892 0.3461 0.076 Uiso 1 1 calc R
C24 C 0.0294(4) 0.1523(2) 0.2836(3) 0.0470(10) Uani 1 1 d .
H24B H 0.1153 0.1717 0.3297 0.071 Uiso 1 1 calc R
H24C H -0.0334 0.1889 0.2495 0.071 Uiso 1 1 calc R
H24A H 0.0430 0.1241 0.2332 0.071 Uiso 1 1 calc R
C25 C 0.9232(4) 0.3871(2) 0.4916(3) 0.0485(11) Uani 1 1 d .
H25C H 0.9602 0.4153 0.4539 0.073 Uiso 1 1 calc R
H25B H 0.8912 0.4162 0.5316 0.073 Uiso 1 1 calc R
H25A H 0.8485 0.3603 0.4443 0.073 Uiso 1 1 calc R
C26 C 0.1207(5) 0.3140(2) 0.3341(3) 0.0487(10) Uani 1 1 d .
H26B H 0.0527 0.2902 0.3492 0.073 Uiso 1 1 calc R
H26C H 0.1869 0.3344 0.3961 0.073 Uiso 1 1 calc R
H26A H 0.1654 0.2818 0.3070 0.073 Uiso 1 1 calc R
Fe1 Fe 0.45632(6) 0.12831(3) 0.70268(5) 0.04200(18) Uani 1 1 d .
N1 N 0.5576(4) 0.04160(17) 0.7667(3) 0.0431(8) Uani 1 1 d .
N2 N 0.4927(3) 0.14953(17) 0.8479(2) 0.0379(7) Uani 1 1 d .
N3 N 0.1911(4) 0.04360(19) 0.6582(3) 0.0452(8) Uani 1 1 d .
N4 N 0.4140(4) 0.09619(18) 0.4831(2) 0.0422(8) Uani 1 1 d .
N5 N 0.2852(4) 0.25643(19) 0.6222(3) 0.0494(9) Uani 1 1 d .
N6 N 0.7255(4) 0.20100(19) 0.7383(3) 0.0451(9) Uani 1 1 d .
N7 N -0.0867(4) 0.08305(18) 0.5345(3) 0.0471(9) Uani 1 1 d .
H7A H -0.0158 0.1030 0.5879 0.057 Uiso 1 1 calc R
N8 N 0.0675(4) 0.05446(19) 0.4053(3) 0.0466(9) Uani 1 1 d .
H8A H 0.1454 0.0767 0.4471 0.056 Uiso 1 1 calc R
Ni1 Ni 0.0000 0.0000 0.5000 0.0455(2) Uani 1 2 d S
O1 O 0.0551(3) 0.36843(16) 0.2578(2) 0.0524(8) Uani 1 1 d .
H1C H 0.1140 0.4005 0.2714 0.063 Uiso 1 1 d R
O2 O 1.0298(3) 0.34062(17) 0.5606(2) 0.0511(8) Uani 1 1 d .
H2A H 1.0698 0.3218 0.5263 0.061 Uiso 1 1 d 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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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
N1 C1 C2 119.9(4) . .
N1 C1 H1 120.0 . .
C2 C1 H1 120.0 . .
C1 C2 C3 119.9(4) . .
C1 C2 H2 120.0 . .
C3 C2 H2 120.0 . .
C2 C3 C4 120.7(4) . .
C2 C3 H3 119.6 . .
C4 C3 H3 119.6 . .
C12 C4 C5 120.3(4) . .
C12 C4 C3 116.9(4) . .
C5 C4 C3 122.8(4) . .
C4 C5 C6 119.9(4) . .
C4 C5 H5 120.1 . .
C6 C5 H5 120.1 . .
C7 C6 C5 119.8(4) . .
C7 C6 H6 120.1 . .
C5 C6 H6 120.1 . .
C11 C7 C6 120.2(4) . .
C11 C7 C8 115.7(3) . .
C6 C7 C8 124.1(4) . .
C9 C8 C7 121.7(4) . .
C9 C8 H8 119.2 . .
C7 C8 H8 119.2 . .
C8 C9 C10 119.4(4) . .
C8 C9 H9 120.3 . .
C10 C9 H9 120.3 . .
N2 C10 C9 120.5(3) . .
N2 C10 H10 119.8 . .
C9 C10 H10 119.8 . .
N2 C11 C7 123.9(4) . .
N2 C11 C12 116.2(4) . .
C7 C11 C12 119.9(4) . .
N1 C12 C4 123.4(4) . .
N1 C12 C11 116.7(4) . .
C4 C12 C11 119.9(4) . .
N3 C13 Fe1 177.3(4) . .
N4 C14 Fe1 176.3(4) . .
N5 C15 Fe1 177.8(4) . .
N6 C16 Fe1 177.3(4) . .
C23 C17 C18 118.4(4) . .
C23 C17 N7 111.8(3) . .
C18 C17 N7 104.0(3) . .
C23 C17 C22 106.0(4) . .
C18 C17 C22 104.5(3) . .
N7 C17 C22 112.0(3) . .
C17 C18 C19 115.2(4) . .
C17 C18 H18A 108.5 . .
C19 C18 H18A 108.5 . .
C17 C18 H18B 108.5 . .
C19 C18 H18B 108.5 . .
H18A C18 H18B 107.5 . .
N8 C19 C24 111.6(3) . .
N8 C19 C18 110.5(3) . .
C24 C19 C18 101.0(3) . .
N8 C19 H19 111.1 . .
C24 C19 H19 111.1 . .
C18 C19 H19 111.1 . .
N8 C20 C21 111.8(4) . .
N8 C20 H20A 109.3 . .
C21 C20 H20A 109.3 . .
N8 C20 H20B 109.3 . .
C21 C20 H20B 109.3 . .
H20A C20 H20B 107.9 . .
N7 C21 C20 106.8(3) 3_556 .
N7 C21 H21A 110.4 3_556 .
C20 C21 H21A 110.4 . .
N7 C21 H21B 110.4 3_556 .
C20 C21 H21B 110.4 . .
H21A C21 H21B 108.6 . .
C17 C22 H22A 109.5 . .
C17 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C17 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
C17 C23 H23A 109.5 . .
C17 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
C17 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
C19 C24 H24B 109.5 . .
C19 C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
C19 C24 H24A 109.5 . .
H24B C24 H24A 109.5 . .
H24C C24 H24A 109.5 . .
O2 C25 H25C 109.5 . .
O2 C25 H25B 109.5 . .
H25C C25 H25B 109.5 . .
O2 C25 H25A 109.5 . .
H25C C25 H25A 109.5 . .
H25B C25 H25A 109.5 . .
O1 C26 H26B 109.5 . .
O1 C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
O1 C26 H26A 109.5 . .
H26B C26 H26A 109.5 . .
H26C C26 H26A 109.5 . .
C15 Fe1 C14 88.88(19) . .
C15 Fe1 C16 93.03(18) . .
C14 Fe1 C16 90.89(17) . .
C15 Fe1 N2 93.58(17) . .
C14 Fe1 N2 176.99(16) . .
C16 Fe1 N2 87.26(15) . .
C15 Fe1 N1 173.95(18) . .
C14 Fe1 N1 95.56(16) . .
C16 Fe1 N1 91.01(16) . .
N2 Fe1 N1 82.10(14) . .
C15 Fe1 C13 90.24(18) . .
C14 Fe1 C13 87.50(16) . .
C16 Fe1 C13 176.33(16) . .
N2 Fe1 C13 94.21(15) . .
N1 Fe1 C13 85.87(15) . .
C12 N1 C1 119.1(3) . .
C12 N1 Fe1 112.4(3) . .
C1 N1 Fe1 128.4(3) . .
C11 N2 C10 118.8(3) . .
C11 N2 Fe1 112.5(3) . .
C10 N2 Fe1 128.6(3) . .
C13 N3 Ni1 136.6(3) . .
C21 N7 C17 112.2(3) 3_556 .
C21 N7 Ni1 107.4(3) 3_556 .
C17 N7 Ni1 124.8(3) . .
C21 N7 H7A 103.3 3_556 .
C17 N7 H7A 103.3 . .
Ni1 N7 H7A 103.3 . .
C20 N8 C19 115.7(3) . .
C20 N8 Ni1 107.5(3) . .
C19 N8 Ni1 112.7(3) . .
C20 N8 H8A 106.8 . .
C19 N8 H8A 106.8 . .
Ni1 N8 H8A 106.8 . .
N7 Ni1 N7 180 . 3_556
N7 Ni1 N8 94.33(15) . .
N7 Ni1 N8 85.67(15) 3_556 .
N7 Ni1 N8 85.67(15) . 3_556
N7 Ni1 N8 94.33(15) 3_556 3_556
N8 Ni1 N8 180 . 3_556
N7 Ni1 N3 78.46(13) . .
N7 Ni1 N3 101.54(13) 3_556 .
N8 Ni1 N3 92.19(13) . .
N8 Ni1 N3 87.81(13) 3_556 .
C26 O1 H1C 105.8 . .
C25 O2 H2A 108.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.387(5) .
C1 C2 1.388(5) .
C1 H1 0.9300 .
C2 C3 1.390(6) .
C2 H2 0.9300 .
C3 C4 1.408(6) .
C3 H3 0.9300 .
C4 C12 1.385(6) .
C4 C5 1.391(6) .
C5 C6 1.391(6) .
C5 H5 0.9300 .
C6 C7 1.390(5) .
C6 H6 0.9300 .
C7 C11 1.387(6) .
C7 C8 1.428(6) .
C8 C9 1.392(5) .
C8 H8 0.9300 .
C9 C10 1.394(6) .
C9 H9 0.9300 .
C10 N2 1.388(5) .
C10 H10 0.9300 .
C11 N2 1.383(5) .
C11 C12 1.393(6) .
C12 N1 1.363(5) .
C13 N3 1.078(5) .
C13 Fe1 2.039(5) .
C14 N4 1.115(5) .
C14 Fe1 1.921(4) .
C15 N5 1.159(5) .
C15 Fe1 1.857(4) .
C16 N6 1.111(5) .
C16 Fe1 1.953(4) .
C17 C23 1.489(5) .
C17 C18 1.516(6) .
C17 N7 1.566(5) .
C17 C22 1.638(6) .
C18 C19 1.563(6) .
C18 H18A 0.9700 .
C18 H18B 0.9700 .
C19 N8 1.463(6) .
C19 C24 1.539(6) .
C19 H19 0.9800 .
C20 N8 1.367(5) .
C20 C21 1.563(6) .
C20 H20A 0.9700 .
C20 H20B 0.9700 .
C21 N7 1.506(6) 3_556
C21 H21A 0.9700 .
C21 H21B 0.9700 .
C22 H22A 0.9600 .
C22 H22B 0.9600 .
C22 H22C 0.9600 .
C23 H23A 0.9600 .
C23 H23B 0.9600 .
C23 H23C 0.9600 .
C24 H24B 0.9600 .
C24 H24C 0.9600 .
C24 H24A 0.9600 .
C25 O2 1.468(5) .
C25 H25C 0.9600 .
C25 H25B 0.9600 .
C25 H25A 0.9600 .
C26 O1 1.467(5) .
C26 H26B 0.9600 .
C26 H26C 0.9600 .
C26 H26A 0.9600 .
Fe1 N2 1.984(3) .
Fe1 N1 2.002(3) .
N3 Ni1 2.486(4) .
N7 C21 1.506(6) 3_556
N7 Ni1 2.017(4) .
N7 H7A 0.9100 .
N8 Ni1 2.065(4) .
N8 H8A 0.9100 .
Ni1 N7 2.017(4) 3_556
Ni1 N8 2.065(4) 3_556
O1 H1C 0.8500 .
O2 H2A 0.8545 .
