#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:55:54 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179431 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/28/4332841.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4332841
loop_
_publ_author_name
'Wen, He-Rui'
'Wang, Cai-Feng'
'Song, You'
'Gao, Song'
'Zuo, Jing-Lin'
'You, Xiao-Zeng'
_publ_section_title
;
 Synthesis, Crystal Structures, and Magnetic Properties of Cyano-Bridged
 Heterobimetallic Chains Based on [(Tp)Fe(CN)3]-
;
_journal_issue                   22
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8942
_journal_page_last               8949
_journal_paper_doi               10.1021/ic060928d
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C26 H28 B2 Fe2 N18 Ni O2, 2(C H4 O)'
_chemical_formula_sum            'C28 H36 B2 Fe2 N18 Ni O4'
_chemical_formula_weight         880.78
_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                 102.767(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.427(3)
_cell_length_b                   11.3692(11)
_cell_length_c                   13.0941(14)
_cell_measurement_reflns_used    2342
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.2
_cell_measurement_theta_min      2.1
_cell_volume                     3982.1(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      293(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     0.71073
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12842
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    1.245
_exptl_absorpt_correction_T_max  0.78
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker(2000)'
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       orange
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         3908
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0452
_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)+(0.07P)²+1.88P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1122
_refine_ls_wR_factor_ref         0.1160
_reflns_number_gt                3071
_reflns_number_total             3908
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060928dsup3.cif
_cod_data_source_block           c2c
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4332841
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
Ni1 Ni 1.0000 0.0000 0.0000 0.02699(16) Uani 1 2 d S
Fe1 Fe 0.874467(16) 0.16519(4) 0.19778(3) 0.03068(15) Uani 1 1 d .
B1 B 0.82207(13) 0.4069(3) 0.1963(3) 0.0334(8) Uani 1 1 d .
H1A H 0.8060 0.4819 0.1961 0.040 Uiso 1 1 d R
C1 C 0.82906(12) 0.2326(3) -0.0300(2) 0.0302(6) Uani 1 1 d .
H1 H 0.8401 0.1669 -0.0606 0.036 Uiso 1 1 calc R
C2 C 0.80050(12) 0.3210(3) -0.0847(3) 0.0363(7) Uani 1 1 d .
H2 H 0.7888 0.3271 -0.1568 0.044 Uiso 1 1 calc R
C3 C 0.79314(11) 0.3979(3) -0.0095(2) 0.0316(7) Uani 1 1 d .
H3 H 0.7747 0.4671 -0.0220 0.038 Uiso 1 1 calc R
C4 C 0.95316(12) 0.3391(3) 0.3123(3) 0.0372(7) Uani 1 1 d .
H4 H 0.9793 0.2859 0.3315 0.045 Uiso 1 1 calc R
C5 C 0.95584(13) 0.4561(3) 0.3370(3) 0.0404(8) Uani 1 1 d .
H5 H 0.9835 0.4972 0.3737 0.049 Uiso 1 1 calc R
C6 C 0.90877(13) 0.5001(3) 0.2959(3) 0.0407(8) Uani 1 1 d .
H6 H 0.8990 0.5778 0.3011 0.049 Uiso 1 1 calc R
C7 C 0.79552(12) 0.1452(3) 0.3317(2) 0.0293(6) Uani 1 1 d .
H7 H 0.8010 0.0668 0.3512 0.035 Uiso 1 1 calc R
C8 C 0.76192(12) 0.2186(3) 0.3635(2) 0.0370(7) Uani 1 1 d .
H8 H 0.7409 0.1999 0.4079 0.044 Uiso 1 1 calc R
C9 C 0.76562(12) 0.3238(3) 0.3169(2) 0.0365(7) Uani 1 1 d .
H9 H 0.7471 0.3908 0.3234 0.044 Uiso 1 1 calc R
C10 C 0.84260(12) 0.0199(3) 0.1419(2) 0.0337(7) Uani 1 1 d .
C11 C 0.91154(11) 0.0841(3) 0.3179(2) 0.0297(6) Uani 1 1 d .
C12 C 0.92754(12) 0.1195(3) 0.1290(3) 0.0351(7) Uani 1 1 d .
C13 C 0.97332(12) 0.2214(3) -0.1349(3) 0.0375(7) Uani 1 1 d .
H14A H 0.9440 0.2235 -0.1061 0.056 Uiso 1 1 calc R
H14B H 0.9651 0.1869 -0.2034 0.056 Uiso 1 1 calc R
H14C H 0.9854 0.3000 -0.1396 0.056 Uiso 1 1 calc R
C14 C 0.88295(15) 0.3359(3) 0.5361(3) 0.0449(9) Uani 1 1 d .
H14D H 0.8791 0.4036 0.5775 0.067 Uiso 1 1 calc R
H14E H 0.8510 0.3134 0.4945 0.067 Uiso 1 1 calc R
H14F H 0.9051 0.3546 0.4911 0.067 Uiso 1 1 calc R
N1 N 0.83886(10) 0.2534(2) 0.0729(2) 0.0354(6) Uani 1 1 d .
N2 N 0.81666(10) 0.3580(2) 0.0857(2) 0.0326(6) Uani 1 1 d .
N3 N 0.90756(10) 0.3121(2) 0.2566(2) 0.0307(6) Uani 1 1 d .
N4 N 0.87923(10) 0.4137(2) 0.2472(2) 0.0340(6) Uani 1 1 d .
N5 N 0.81919(10) 0.2042(2) 0.26809(19) 0.0310(6) Uani 1 1 d .
N6 N 0.80011(10) 0.3148(2) 0.2607(2) 0.0323(6) Uani 1 1 d .
N7 N 0.82572(10) -0.0668(2) 0.1057(2) 0.0322(6) Uani 1 1 d .
N8 N 0.95695(10) 0.0848(2) 0.0867(2) 0.0309(6) Uani 1 1 d .
N9 N 0.93763(10) 0.0396(2) 0.3893(2) 0.0325(6) Uani 1 1 d .
O1 O 1.00869(8) 0.15716(18) -0.07282(17) 0.0353(5) Uani 1 1 d .
H1D H 1.0301 0.1436 -0.1093 0.042 Uiso 1 1 d R
O2 O 0.90311(9) 0.2419(2) 0.6029(2) 0.0440(6) Uani 1 1 d .
H2B H 0.8829 0.1842 0.5932 0.066 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'
B B 0.0013 0.0007 '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
N9 Ni1 N9 180.00(18) 2_755 6
N9 Ni1 N8 89.88(10) 2_755 .
N9 Ni1 N8 90.12(10) 6 .
N9 Ni1 N8 90.12(10) 2_755 5_755
N9 Ni1 N8 89.88(10) 6 5_755
N8 Ni1 N8 180.00(13) . 5_755
N9 Ni1 O1 91.57(10) 2_755 5_755
N9 Ni1 O1 88.43(10) 6 5_755
N8 Ni1 O1 90.68(10) . 5_755
N8 Ni1 O1 89.32(10) 5_755 5_755
N9 Ni1 O1 88.43(10) 2_755 .
N9 Ni1 O1 91.57(10) 6 .
N8 Ni1 O1 89.32(10) . .
N8 Ni1 O1 90.68(10) 5_755 .
O1 Ni1 O1 180.00(16) 5_755 .
C11 Fe1 C10 90.76(13) . .
C11 Fe1 C12 86.31(13) . .
C10 Fe1 C12 85.33(13) . .
C11 Fe1 N3 88.38(12) . .
C10 Fe1 N3 179.14(12) . .
C12 Fe1 N3 94.60(12) . .
C11 Fe1 N1 177.36(12) . .
C10 Fe1 N1 91.20(12) . .
C12 Fe1 N1 92.08(12) . .
N3 Fe1 N1 89.66(11) . .
C11 Fe1 N5 92.75(12) . .
C10 Fe1 N5 92.21(12) . .
C12 Fe1 N5 177.36(12) . .
N3 Fe1 N5 87.84(11) . .
N1 Fe1 N5 88.96(11) . .
N2 B1 N6 107.6(3) . .
N2 B1 N4 107.5(3) . .
N6 B1 N4 106.0(2) . .
N2 B1 H1A 111.9 . .
N6 B1 H1A 111.6 . .
N4 B1 H1A 112.0 . .
N1 C1 C2 111.1(3) . .
N1 C1 H1 124.4 . .
C2 C1 H1 124.4 . .
C3 C2 C1 104.5(3) . .
C3 C2 H2 127.7 . .
C1 C2 H2 127.7 . .
N2 C3 C2 109.6(3) . .
N2 C3 H3 125.2 . .
C2 C3 H3 125.2 . .
N3 C4 C5 110.3(3) . .
N3 C4 H4 124.8 . .
C5 C4 H4 124.8 . .
C4 C5 C6 105.3(3) . .
C4 C5 H5 127.3 . .
C6 C5 H5 127.3 . .
N4 C6 C5 109.6(3) . .
N4 C6 H6 125.2 . .
C5 C6 H6 125.2 . .
N5 C7 C8 109.5(3) . .
N5 C7 H7 125.3 . .
C8 C7 H7 125.3 . .
C9 C8 C7 106.1(3) . .
C9 C8 H8 127.0 . .
C7 C8 H8 127.0 . .
N6 C9 C8 108.4(3) . .
N6 C9 H9 125.8 . .
C8 C9 H9 125.8 . .
N7 C10 Fe1 176.2(3) . .
N9 C11 Fe1 174.2(3) . .
N8 C12 Fe1 174.9(3) . .
O1 C13 H14A 109.5 . .
O1 C13 H14B 109.5 . .
H14A C13 H14B 109.5 . .
O1 C13 H14C 109.5 . .
H14A C13 H14C 109.5 . .
H14B C13 H14C 109.5 . .
O2 C14 H14D 109.5 . .
O2 C14 H14E 109.5 . .
H14D C14 H14E 109.5 . .
O2 C14 H14F 109.5 . .
H14D C14 H14F 109.5 . .
H14E C14 H14F 109.5 . .
C1 N1 N2 106.4(2) . .
C1 N1 Fe1 134.1(2) . .
N2 N1 Fe1 119.5(2) . .
C3 N2 N1 108.4(3) . .
C3 N2 B1 132.9(3) . .
N1 N2 B1 118.7(2) . .
C4 N3 N4 107.2(3) . .
C4 N3 Fe1 134.5(2) . .
N4 N3 Fe1 118.13(19) . .
C6 N4 N3 107.5(3) . .
C6 N4 B1 133.0(3) . .
N3 N4 B1 119.2(3) . .
C7 N5 N6 106.0(3) . .
C7 N5 Fe1 134.2(2) . .
N6 N5 Fe1 119.7(2) . .
C9 N6 N5 110.1(3) . .
C9 N6 B1 131.5(3) . .
N5 N6 B1 118.4(3) . .
C12 N8 Ni1 169.6(3) . .
C11 N9 Ni1 160.5(3) . 2_755
C13 O1 Ni1 127.7(2) . .
C13 O1 H1D 104.9 . .
Ni1 O1 H1D 105.6 . .
C14 O2 H2B 109.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N9 2.033(3) 2_755
Ni1 N9 2.033(3) 6
Ni1 N8 2.050(3) .
Ni1 N8 2.050(3) 5_755
Ni1 O1 2.064(2) 5_755
Ni1 O1 2.064(2) .
Fe1 C11 1.911(3) .
Fe1 C10 1.935(3) .
Fe1 C12 1.944(4) .
Fe1 N3 1.974(3) .
Fe1 N1 1.981(3) .
Fe1 N5 1.990(3) .
B1 N2 1.528(4) .
B1 N6 1.547(5) .
B1 N4 1.564(4) .
B1 H1A 0.9600 .
C1 N1 1.336(4) .
C1 C2 1.375(4) .
C1 H1 0.9300 .
C2 C3 1.364(5) .
C2 H2 0.9300 .
C3 N2 1.349(4) .
C3 H3 0.9300 .
C4 N3 1.337(4) .
C4 C5 1.366(5) .
C4 H4 0.9300 .
C5 C6 1.378(5) .
C5 H5 0.9300 .
C6 N4 1.341(4) .
C6 H6 0.9300 .
C7 N5 1.343(4) .
C7 C8 1.374(5) .
C7 H7 0.9300 .
C8 C9 1.357(5) .
C8 H8 0.9300 .
C9 N6 1.325(4) .
C9 H9 0.9300 .
C10 N7 1.147(4) .
C11 N9 1.160(4) .
C12 N8 1.145(4) .
C13 O1 1.337(4) .
C13 H14A 0.9600 .
C13 H14B 0.9600 .
C13 H14C 0.9600 .
C14 O2 1.414(4) .
C14 H14D 0.9600 .
C14 H14E 0.9600 .
C14 H14F 0.9600 .
N1 N2 1.364(4) .
N3 N4 1.382(4) .
N5 N6 1.357(4) .
N9 Ni1 2.033(3) 2_755
O1 H1D 0.8500 .
O2 H2B 0.8501 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1D O2 0.85 2.13 2.713(3) 125.4 2_755
O2 H2B N7 0.85 2.09 2.916(4) 162.8 6_556
