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#$Date: 2016-10-08 01:33:12 +0300 (Sat, 08 Oct 2016) $
#$Revision: 187162 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/57/7055718.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_7055718
loop_
_publ_author_name
'Dong, Dapeng'
'Zhang, Yanjuan'
'Jiao, Chengqi'
'Zhao, Liang'
'Liu, Tao'
'Liu, Dedi'
'Li, Zhenghua'
'Liu, Jia'
'Liu, Dongping'
_publ_section_title
;
 Syntheses, structures, and magnetic properties of three new cyano-bridged
 heterobimetallic chains based on [Fe(Tp*)(CN)3]−
;
_journal_issue                   10
_journal_name_full               'New J. Chem.'
_journal_page_first              8451
_journal_paper_doi               10.1039/C6NJ01015F
_journal_volume                  40
_journal_year                    2016
_chemical_formula_sum            'C40 H60 B2 Co Fe2 N18 O6'
_chemical_formula_weight         1081.31
_space_group_crystal_system      orthorhombic
_space_group_IT_number           72
_space_group_name_Hall           '-I 2 2c'
_space_group_name_H-M_alt        'I b a m'
_symmetry_space_group_name_Hall  '-I 2 2c'
_symmetry_space_group_name_H-M   'I b a m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-08-07 deposited with the CCDC.
2016-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.022(9)
_cell_length_b                   26.818(17)
_cell_length_c                   13.992(9)
_cell_measurement_reflns_used    2043
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      21.16
_cell_measurement_theta_min      2.50
_cell_volume                     5637(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0776
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12378
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.503
_exptl_absorpt_coefficient_mu    0.855
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_description       needle
_exptl_crystal_F_000             2252
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.075
_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     174
_refine_ls_number_reflns         2525
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1047P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1642
_refine_ls_wR_factor_ref         0.1757
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1757
_reflns_number_total             2525
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6nj01015f2.cif
_cod_data_source_block           1_sq
_cod_depositor_comments
'Adding full bibliography for 7055717--7055719.cif.'
_cod_database_code               7055718
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1, y+1, -z+1/2'
'x+1, -y+1, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z'
'-x-1/2, y-1/2, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x, -y, z+1/2'
'-x, y, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Fe1 Fe 0.55291(5) 0.36355(3) 0.0000 0.0391(3) Uani 1 2 d S T P
Co1 Co 0.5000 0.5000 0.2500 0.0410(4) Uani 1 4 d S T P
N1 N 0.4306(3) 0.28026(18) 0.0000 0.0457(13) Uani 1 2 d S T P
N2 N 0.4344(3) 0.33143(18) 0.0000 0.0436(12) Uani 1 2 d S T P
N3 N 0.5717(2) 0.26671(13) 0.0882(3) 0.0464(9) Uani 1 1 d . . .
N4 N 0.5907(2) 0.31573(13) 0.1019(2) 0.0445(9) Uani 1 1 d . . .
N5 N 0.5044(2) 0.44474(13) 0.1443(3) 0.0509(9) Uani 1 1 d . . .
N6 N 0.7376(5) 0.4110(3) 0.0000 0.098(3) Uani 1 2 d S T P
C1 C 0.3228(5) 0.2111(3) 0.0000 0.077(2) Uani 1 2 d S T P
H1C H 0.2592 0.2078 0.0000 0.116 Uiso 1 2 d R U P
H1D H 0.3468 0.1954 -0.0560 0.116 Uiso 0.5 1 d R U P
C2 C 0.3465(4) 0.2644(3) 0.0000 0.0533(16) Uani 1 2 d S T P
C3 C 0.2938(4) 0.3054(3) 0.0000 0.0587(18) Uani 1 2 d S T P
H3A H 0.2319 0.3059 0.0000 0.070 Uiso 1 2 calc R U P
C4 C 0.3498(4) 0.3464(3) 0.0000 0.0531(17) Uani 1 2 d S T P
C5 C 0.3210(4) 0.4004(3) 0.0000 0.0647(19) Uani 1 2 d S T P
H5A H 0.3732 0.4210 0.0000 0.097 Uiso 1 2 d R U P
H5B H 0.2862 0.4073 -0.0560 0.097 Uiso 0.5 1 d R U P
C6 C 0.5929(4) 0.1845(2) 0.1669(5) 0.089(2) Uani 1 1 d . . .
H6A H 0.6180 0.1722 0.2255 0.134 Uiso 1 1 calc R U .
H6B H 0.5310 0.1756 0.1639 0.134 Uiso 1 1 calc R U .
H6C H 0.6238 0.1700 0.1137 0.134 Uiso 1 1 calc R U .
C7 C 0.6020(3) 0.24049(18) 0.1634(4) 0.0564(12) Uani 1 1 d . . .
C8 C 0.6401(3) 0.2734(2) 0.2260(4) 0.0649(14) Uani 1 1 d . . .
H8A H 0.6660 0.2657 0.2846 0.078 Uiso 1 1 calc R U .
C9 C 0.6330(3) 0.31915(19) 0.1863(3) 0.0554(13) Uani 1 1 d . . .
C10 C 0.6666(4) 0.3668(2) 0.2278(4) 0.0788(17) Uani 1 1 d . . .
H10A H 0.6944 0.3603 0.2882 0.118 Uiso 1 1 calc R U .
H10B H 0.7092 0.3814 0.1850 0.118 Uiso 1 1 calc R U .
H10C H 0.6178 0.3895 0.2367 0.118 Uiso 1 1 calc R U .
C11 C 0.5202(3) 0.41310(15) 0.0922(3) 0.0434(10) Uani 1 1 d . . .
C12 C 0.6703(5) 0.3936(2) 0.0000 0.0593(18) Uani 1 2 d S T P
O1 O 0.3602(3) 0.5000 0.2500 0.0715(14) Uani 1 2 d S T P
B1 B 0.5180(5) 0.2509(3) 0.0000 0.0477(17) Uani 1 2 d S T P
C13 C 0.3040(9) 0.4992(5) 0.1770(12) 0.108(5) Uani 0.5 1 d . . P
H13A H 0.3121 0.4638 0.1656 0.129 Uiso 0.5 1 d R U P
H13B H 0.3461 0.5144 0.1333 0.129 Uiso 0.5 1 d R U P
C14 C 0.2315(9) 0.5031(5) 0.1093(10) 0.100(4) Uani 0.5 1 d . . P
H14A H 0.2483 0.4884 0.0494 0.149 Uiso 0.5 1 d R U P
H14B H 0.1806 0.4858 0.1346 0.149 Uiso 0.5 1 d R U P
H14C H 0.2169 0.5376 0.0999 0.149 Uiso 0.5 1 d R U P
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'
Co Co 0.3494 0.9721 '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
C11 Fe1 C11 84.6(2) 10 .
C11 Fe1 C12 86.88(19) 10 .
C11 Fe1 C12 86.88(19) . .
C11 Fe1 N2 94.06(17) 10 .
C11 Fe1 N2 94.06(17) . .
C12 Fe1 N2 178.7(2) . .
C11 Fe1 N4 92.17(16) 10 10
C11 Fe1 N4 175.94(16) . 10
C12 Fe1 N4 90.48(17) . 10
N2 Fe1 N4 88.62(14) . 10
C11 Fe1 N4 175.94(16) 10 .
C11 Fe1 N4 92.17(16) . .
C12 Fe1 N4 90.48(17) . .
N2 Fe1 N4 88.62(14) . .
N4 Fe1 N4 90.9(2) 10 .
N5 Co1 N5 176.4(2) . 8_455
N5 Co1 N5 89.9(2) . 7_545
N5 Co1 N5 90.2(2) 8_455 7_545
N5 Co1 N5 90.2(2) . 2_665
N5 Co1 N5 89.9(2) 8_455 2_665
N5 Co1 N5 176.4(2) 7_545 2_665
N5 Co1 O1 91.79(10) . .
N5 Co1 O1 91.79(10) 8_455 .
N5 Co1 O1 88.21(10) 7_545 .
N5 Co1 O1 88.21(10) 2_665 .
N5 Co1 O1 88.21(10) . 2_665
N5 Co1 O1 88.21(10) 8_455 2_665
N5 Co1 O1 91.79(10) 7_545 2_665
N5 Co1 O1 91.79(10) 2_665 2_665
O1 Co1 O1 180.0 . 2_665
C2 N1 N2 111.0(5) . .
C2 N1 B1 130.4(5) . .
N2 N1 B1 118.6(5) . .
C4 N2 N1 105.2(5) . .
C4 N2 Fe1 136.6(5) . .
N1 N2 Fe1 118.2(3) . .
C7 N3 N4 109.0(4) . .
C7 N3 B1 131.5(4) . .
N4 N3 B1 119.4(4) . .
C9 N4 N3 106.8(3) . .
C9 N4 Fe1 135.8(3) . .
N3 N4 Fe1 117.5(3) . .
C11 N5 Co1 169.0(4) . .
C2 C1 H1C 109.2 . .
C2 C1 H1D 109.6 . .
H1C C1 H1D 109.5 . .
N1 C2 C3 107.1(6) . .
N1 C2 C1 122.6(6) . .
C3 C2 C1 130.3(6) . .
C2 C3 C4 106.8(6) . .
C2 C3 H3A 126.6 . .
C4 C3 H3A 126.6 . .
N2 C4 C3 109.9(6) . .
N2 C4 C5 124.2(6) . .
C3 C4 C5 125.9(6) . .
C4 C5 H5A 108.5 . .
C4 C5 H5B 110.0 . .
H5A C5 H5B 109.5 . .
C7 C6 H6A 109.5 . .
C7 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C7 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
N3 C7 C8 107.8(4) . .
N3 C7 C6 121.0(5) . .
C8 C7 C6 131.2(5) . .
C9 C8 C7 106.8(4) . .
C9 C8 H8A 126.6 . .
C7 C8 H8A 126.6 . .
N4 C9 C8 109.7(4) . .
N4 C9 C10 124.1(4) . .
C8 C9 C10 126.2(4) . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
N5 C11 Fe1 175.6(4) . .
N6 C12 Fe1 179.7(7) . .
C13 O1 C13 100.8(13) . 8_455
C13 O1 Co1 129.6(7) . .
C13 O1 Co1 129.6(7) 8_455 .
N1 B1 N3 108.0(3) . 10
N1 B1 N3 108.0(3) . .
N3 B1 N3 107.1(5) 10 .
O1 C13 C14 169.3(13) . .
O1 C13 H13A 93.6 . .
C14 C13 H13A 93.3 . .
O1 C13 H13B 93.7 . .
C14 C13 H13B 92.7 . .
H13A C13 H13B 103.0 . .
C13 C14 H14A 110.2 . .
C13 C14 H14B 108.9 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.4 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 C11 1.916(5) 10
Fe1 C11 1.916(5) .
Fe1 C12 1.939(8) .
Fe1 N2 1.978(5) .
Fe1 N4 1.999(3) 10
Fe1 N4 1.999(3) .
Co1 N5 2.095(4) .
Co1 N5 2.095(4) 8_455
Co1 N5 2.095(4) 7_545
Co1 N5 2.095(4) 2_665
Co1 O1 2.099(5) .
Co1 O1 2.099(5) 2_665
N1 C2 1.333(7) .
N1 N2 1.373(6) .
N1 B1 1.531(8) .
N2 C4 1.332(7) .
N3 C7 1.345(5) .
N3 N4 1.359(5) .
N3 B1 1.535(5) .
N4 C9 1.345(5) .
N5 C11 1.144(5) .
N6 C12 1.114(9) .
C1 C2 1.473(9) .
C1 H1C 0.9600 .
C1 H1D 0.9599 .
C2 C3 1.355(9) .
C3 C4 1.385(9) .
C3 H3A 0.9300 .
C4 C5 1.511(9) .
C5 H5A 0.9599 .
C5 H5B 0.9600 .
C6 C7 1.510(7) .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C7 C8 1.369(7) .
C8 C9 1.351(6) .
C8 H8A 0.9300 .
C9 C10 1.492(7) .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
O1 C13 1.326(16) .
O1 C13 1.326(16) 8_455
B1 N3 1.535(5) 10
C13 C14 1.447(18) .
C13 H13A 0.9700 .
C13 H13B 0.9699 .
C14 H14A 0.9599 .
C14 H14B 0.9601 .
C14 H14C 0.9599 .
