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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/7/05/57/7055719.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_7055719
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 Fe3 N18 O6'
_chemical_formula_weight         1078.23
_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                   14.97(2)
_cell_length_b                   27.32(4)
_cell_length_c                   14.14(2)
_cell_measurement_reflns_used    1197
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      21.73
_cell_measurement_theta_min      2.48
_cell_volume                     5783(14)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.1245
_diffrn_reflns_av_unetI/netI     0.0968
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13030
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.479
_exptl_absorpt_coefficient_mu    0.797
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       needle
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2643
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0712P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1421
_refine_ls_wR_factor_ref         0.1618
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1651
_reflns_number_total             2643
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6nj01015f2.cif
_cod_data_source_block           2_sq
_cod_depositor_comments
'Adding full bibliography for 7055717--7055719.cif.'
_cod_original_cell_volume        5785(15)
_cod_database_code               7055719
_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 0.5000 0.5000 0.7500 0.0390(4) Uani 1 4 d S T P
Fe2 Fe 0.44563(5) 0.63731(3) 1.0000 0.0373(3) Uani 1 2 d S T P
N1 N 0.5675(3) 0.72015(18) 1.0000 0.0390(13) Uani 1 2 d S T P
N2 N 0.5655(3) 0.66921(18) 1.0000 0.0394(13) Uani 1 2 d S T P
N3 N 0.4256(2) 0.73320(13) 0.9120(3) 0.0412(9) Uani 1 1 d . . .
N4 N 0.4064(2) 0.68427(12) 0.8982(2) 0.0392(9) Uani 1 1 d . . .
N5 N 0.4959(2) 0.55656(14) 0.8572(3) 0.0448(9) Uani 1 1 d . . .
N6 N 0.2572(4) 0.5905(3) 1.0000 0.083(2) Uani 1 2 d S T P
C1 C 0.6787(4) 0.6013(2) 1.0000 0.0560(19) Uani 1 2 d S T P
H1B H 0.6314 0.5752 1.0000 0.084 Uiso 1 2 d R U P
H1C H 0.7187 0.5886 0.9446 0.084 Uiso 0.5 1 d R U P
C2 C 0.6507(4) 0.6543(2) 1.0000 0.0425(16) Uani 1 2 d S T P
C3 C 0.7081(4) 0.6958(2) 1.0000 0.0487(17) Uani 1 2 d S T P
H3A H 0.7703 0.6957 1.0000 0.058 Uiso 1 2 calc R U P
C4 C 0.6533(4) 0.7362(2) 1.0000 0.0441(16) Uani 1 2 d S T P
C5 C 0.6785(5) 0.7890(2) 1.0000 0.066(2) Uani 1 2 d S T P
H5A H 0.6251 0.8085 1.0000 0.100 Uiso 1 2 d R U P
H5B H 0.7130 0.7963 1.0554 0.100 Uiso 0.5 1 d R U P
C6 C 0.4060(4) 0.81420(18) 0.8296(4) 0.0727(17) Uani 1 1 d . . .
H6A H 0.4350 0.8260 0.8856 0.109 Uiso 1 1 calc R U .
H6B H 0.4412 0.8226 0.7752 0.109 Uiso 1 1 calc R U .
H6C H 0.3480 0.8289 0.8243 0.109 Uiso 1 1 calc R U .
C7 C 0.3964(3) 0.75917(18) 0.8354(4) 0.0517(13) Uani 1 1 d . . .
C8 C 0.3597(3) 0.7266(2) 0.7731(4) 0.0608(15) Uani 1 1 d . . .
H8A H 0.3351 0.7341 0.7145 0.073 Uiso 1 1 calc R U .
C9 C 0.3659(3) 0.68035(18) 0.8129(3) 0.0487(12) Uani 1 1 d . . .
C10 C 0.3330(4) 0.6340(2) 0.7721(4) 0.0722(17) Uani 1 1 d . . .
H10A H 0.3069 0.6403 0.7113 0.108 Uiso 1 1 calc R U .
H10B H 0.3819 0.6116 0.7652 0.108 Uiso 1 1 calc R U .
H10C H 0.2888 0.6201 0.8133 0.108 Uiso 1 1 calc R U .
C11 C 0.4792(3) 0.58821(16) 0.9093(3) 0.0404(11) Uani 1 1 d . . .
C12 C 0.3267(5) 0.6072(2) 1.0000 0.0534(18) Uani 1 2 d S T P
O1 O 0.6431(3) 0.5000 0.7500 0.0610(13) Uani 1 2 d S T P
B1 B 0.4797(5) 0.7488(3) 1.0000 0.0445(19) Uani 1 2 d S T P
C13 C 0.6996(8) 0.5004(4) 0.8228(9) 0.076(3) Uani 0.5 1 d . . P
H13A H 0.6573 0.4827 0.8621 0.091 Uiso 0.5 1 d R U P
H13B H 0.6864 0.5343 0.8370 0.091 Uiso 0.5 1 d R U P
C14 C 0.7653(7) 0.4980(4) 0.8958(10) 0.084(4) Uani 0.5 1 d . . P
H14A H 0.7415 0.5097 0.9547 0.127 Uiso 0.5 1 d R U P
H14B H 0.7850 0.4647 0.9033 0.127 Uiso 0.5 1 d R U P
H14C H 0.8150 0.5180 0.8773 0.127 Uiso 0.5 1 d R U P
H1A H 0.489(3) 0.793(2) 1.0000 0.045(16) Uiso 1 2 d S . 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'
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
O1 Fe1 O1 180.0 2_665 .
O1 Fe1 N5 88.39(9) 2_665 .
O1 Fe1 N5 91.61(9) . .
O1 Fe1 N5 88.39(9) 2_665 8_456
O1 Fe1 N5 91.61(9) . 8_456
N5 Fe1 N5 176.78(18) . 8_456
O1 Fe1 N5 91.61(9) 2_665 2_665
O1 Fe1 N5 88.39(9) . 2_665
N5 Fe1 N5 91.1(2) . 2_665
N5 Fe1 N5 89.0(2) 8_456 2_665
O1 Fe1 N5 91.61(9) 2_665 7_546
O1 Fe1 N5 88.39(9) . 7_546
N5 Fe1 N5 89.0(2) . 7_546
N5 Fe1 N5 91.1(2) 8_456 7_546
N5 Fe1 N5 176.78(18) 2_665 7_546
C11 Fe2 C11 83.7(3) . 10_557
C11 Fe2 C12 86.8(2) . .
C11 Fe2 C12 86.8(2) 10_557 .
C11 Fe2 N2 94.00(18) . .
C11 Fe2 N2 94.00(18) 10_557 .
C12 Fe2 N2 178.9(2) . .
C11 Fe2 N4 92.5(2) . .
C11 Fe2 N4 175.27(16) 10_557 .
C12 Fe2 N4 90.15(18) . .
N2 Fe2 N4 89.07(16) . .
C11 Fe2 N4 175.27(16) . 10_557
C11 Fe2 N4 92.5(2) 10_557 10_557
C12 Fe2 N4 90.15(18) . 10_557
N2 Fe2 N4 89.07(16) . 10_557
N4 Fe2 N4 91.1(2) . 10_557
C4 N1 N2 110.1(5) . .
C4 N1 B1 130.4(6) . .
N2 N1 B1 119.5(5) . .
C2 N2 N1 106.4(5) . .
C2 N2 Fe2 136.4(4) . .
N1 N2 Fe2 117.2(3) . .
C7 N3 N4 108.9(4) . .
C7 N3 B1 131.6(5) . .
N4 N3 B1 119.3(4) . .
C9 N4 N3 107.2(4) . .
C9 N4 Fe2 135.7(3) . .
N3 N4 Fe2 117.1(3) . .
C11 N5 Fe1 168.5(3) . .
C2 C1 H1B 119.1 . .
C2 C1 H1C 118.6 . .
H1B C1 H1C 99.6 . .
N2 C2 C3 109.5(5) . .
N2 C2 C1 123.8(6) . .
C3 C2 C1 126.7(6) . .
C4 C3 C2 106.1(6) . .
C4 C3 H3A 126.9 . .
C2 C3 H3A 126.9 . .
N1 C4 C3 107.9(6) . .
N1 C4 C5 123.4(6) . .
C3 C4 C5 128.7(6) . .
C4 C5 H5A 109.1 . .
C4 C5 H5B 109.7 . .
H5A C5 H5B 109.4 . .
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 . .
C8 C7 N3 107.6(4) . .
C8 C7 C6 130.6(5) . .
N3 C7 C6 121.9(5) . .
C7 C8 C9 107.7(5) . .
C7 C8 H8A 126.1 . .
C9 C8 H8A 126.1 . .
N4 C9 C8 108.7(4) . .
N4 C9 C10 124.5(4) . .
C8 C9 C10 126.9(5) . .
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 Fe2 175.8(4) . .
N6 C12 Fe2 178.9(7) . .
C13 O1 C13 101.2(11) 8_456 .
C13 O1 Fe1 129.4(6) 8_456 .
C13 O1 Fe1 129.4(6) . .
N1 B1 N3 108.0(4) . .
N1 B1 N3 108.0(4) . 10_557
N3 B1 N3 107.4(5) . 10_557
N1 B1 H1A 114(2) . .
N3 B1 H1A 109.4(13) . .
N3 B1 H1A 109.4(13) 10_557 .
O1 C13 C14 174.8(12) . .
O1 C13 H13A 91.4 . .
C14 C13 H13A 90.7 . .
O1 C13 H13B 92.1 . .
C14 C13 H13B 92.0 . .
H13A C13 H13B 103.0 . .
C13 C14 H14A 110.8 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 108.1 . .
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 O1 2.143(6) 2_665
Fe1 O1 2.143(6) .
Fe1 N5 2.166(5) .
Fe1 N5 2.166(5) 8_456
Fe1 N5 2.166(5) 2_665
Fe1 N5 2.166(5) 7_546
Fe2 C11 1.923(5) .
Fe2 C11 1.923(5) 10_557
Fe2 C12 1.961(8) .
Fe2 N2 1.995(5) .
Fe2 N4 2.015(4) .
Fe2 N4 2.015(4) 10_557
N1 C4 1.357(7) .
N1 N2 1.392(7) .
N1 B1 1.531(8) .
N2 C2 1.339(7) .
N3 C7 1.367(6) .
N3 N4 1.381(5) .
N3 B1 1.544(6) .
N4 C9 1.355(6) .
N5 C11 1.163(5) .
N6 C12 1.136(9) .
C1 C2 1.507(8) .
C1 H1B 1.0053 .
C1 H1C 1.0466 .
C2 C3 1.423(9) .
C3 C4 1.374(9) .
C3 H3A 0.9300 .
C4 C5 1.492(9) .
C5 H5A 0.9603 .
C5 H5B 0.9602 .
C6 C7 1.513(7) .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C7 C8 1.367(7) .
C8 C9 1.387(7) .
C8 H8A 0.9300 .
C9 C10 1.476(7) .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
O1 C13 1.332(12) 8_456
O1 C13 1.332(12) .
B1 N3 1.544(6) 10_557
B1 H1A 1.22(5) .
C13 C14 1.428(15) .
C13 H13A 0.9700 .
C13 H13B 0.9698 .
C14 H14A 0.9601 .
C14 H14B 0.9599 .
C14 H14C 0.9602 .
