#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:32:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179115 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/77/4307769.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_4307769
loop_
_publ_author_name
'Zhi-Guo Gu'
'Wei Liu'
'Qiao-Fang Yang'
'Xin-Hui Zhou'
'Jing-Lin Zuo'
'Xiao-Zeng You'
_publ_section_title
;
Cyano-Bridged FeIII2CuII3 and FeIII4NiII4 Complexes: Syntheses, Structures,
and Magnetic Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3236
_journal_page_last               3244
_journal_paper_doi               10.1021/ic062267q
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C17 H15 B Fe N11 O3 Zn'
_chemical_formula_weight         553.43
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.4420(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5235(2)
_cell_length_b                   12.4295(2)
_cell_length_c                   15.7847(2)
_cell_measurement_reflns_used    3088
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      2.1
_cell_volume                     2250.67(6)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Aepex CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22732
_diffrn_reflns_theta_full        28.23
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    1.755
_exptl_absorpt_correction_T_max  0.67
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, (Bruker, 2000)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         5564
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0296
_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)+(0.0436P)²+0.8158P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0836
_reflns_number_gt                4493
_reflns_number_total             5564
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062267qsi20061128_104054.cif
_cod_data_source_block           50502bm
_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_database_code               4307769
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.76009(2) 0.70584(2) -0.001674(16) 0.02619(8) Uani 1 1 d . . .
Zn1 Zn 0.93688(2) 0.41219(2) 0.189440(15) 0.03430(8) Uani 1 1 d . . .
B1 B 0.50271(19) 0.77678(17) -0.03704(14) 0.0284(4) Uani 1 1 d . . .
N1 N 0.69957(14) 0.82270(13) -0.07782(10) 0.0297(3) Uani 1 1 d . . .
N2 N 0.58343(14) 0.84546(13) -0.08836(10) 0.0295(3) Uani 1 1 d . . .
N3 N 0.66173(14) 0.75885(14) 0.08352(10) 0.0302(3) Uani 1 1 d . . .
N4 N 0.54965(14) 0.78471(13) 0.05831(10) 0.0296(3) Uani 1 1 d . . .
N5 N 0.62937(14) 0.61663(13) -0.05015(10) 0.0273(3) Uani 1 1 d . . .
N6 N 0.51992(13) 0.65867(13) -0.06509(10) 0.0270(3) Uani 1 1 d . . .
N7 N 0.85496(17) 0.52362(16) 0.11493(12) 0.0437(5) Uani 1 1 d . . .
N8 N 0.95167(18) 0.85652(18) 0.07678(14) 0.0524(5) Uani 1 1 d . . .
N9 N 1.06988(17) 0.37231(16) 0.12594(12) 0.0433(4) Uani 1 1 d . . .
N10 N 0.37767(15) 0.81204(14) -0.04632(12) 0.0377(4) Uani 1 1 d . . .
N11 N 0.29339(17) 0.7408(2) -0.02633(16) 0.0569(6) Uani 1 1 d . . .
O1 O 0.99310(18) 0.49700(15) 0.29019(11) 0.0597(5) Uani 1 1 d . . .
O2 O 0.81612(17) 0.32487(14) 0.23033(12) 0.0562(5) Uani 1 1 d . . .
O3 O 0.94478(18) 0.19613(15) 0.22314(14) 0.0624(5) Uani 1 1 d . . .
C1 C 0.7514(2) 0.88515(18) -0.13174(13) 0.0378(5) Uani 1 1 d . . .
H1 H 0.8310 0.8862 -0.1372 0.045 Uiso 1 1 calc R . .
C2 C 0.6695(2) 0.94806(18) -0.17829(14) 0.0429(5) Uani 1 1 d . . .
H2 H 0.6828 0.9984 -0.2199 0.051 Uiso 1 1 calc R . .
C3 C 0.5648(2) 0.92066(16) -0.15017(14) 0.0377(5) Uani 1 1 d . . .
H3 H 0.4927 0.9490 -0.1702 0.045 Uiso 1 1 calc R . .
C4 C 0.6777(2) 0.77375(19) 0.16766(13) 0.0408(5) Uani 1 1 d . . .
H4 H 0.7473 0.7619 0.2012 0.049 Uiso 1 1 calc R . .
C5 C 0.5756(2) 0.8093(2) 0.19731(15) 0.0484(6) Uani 1 1 d . . .
H5 H 0.5632 0.8260 0.2532 0.058 Uiso 1 1 calc R . .
C6 C 0.4961(2) 0.81497(17) 0.12673(14) 0.0388(5) Uani 1 1 d . . .
H6 H 0.4186 0.8361 0.1263 0.047 Uiso 1 1 calc R . .
C7 C 0.62369(19) 0.51585(16) -0.08019(13) 0.0341(4) Uani 1 1 d . . .
H7 H 0.6859 0.4679 -0.0772 0.041 Uiso 1 1 calc R . .
C8 C 0.51300(19) 0.49317(17) -0.11600(13) 0.0367(5) Uani 1 1 d . . .
H8 H 0.4866 0.4294 -0.1419 0.044 Uiso 1 1 calc R . .
C9 C 0.44946(18) 0.58527(16) -0.10519(13) 0.0328(4) Uani 1 1 d . . .
H9 H 0.3708 0.5949 -0.1228 0.039 Uiso 1 1 calc R . .
C10 C 0.86443(17) 0.65575(16) -0.08098(13) 0.0328(4) Uani 1 1 d . . .
C11 C 0.88414(19) 0.79722(17) 0.04652(14) 0.0366(5) Uani 1 1 d . . .
C12 C 0.82020(18) 0.59158(17) 0.07127(13) 0.0334(4) Uani 1 1 d . . .
C13 C 0.3354(3) 0.9145(2) -0.04700(18) 0.0552(7) Uani 1 1 d . . .
H13 H 0.3757 0.9773 -0.0572 0.066 Uiso 1 1 calc R . .
C14 C 0.2213(3) 0.9064(3) -0.0297(2) 0.0744(10) Uani 1 1 d . . .
H14 H 0.1688 0.9628 -0.0267 0.089 Uiso 1 1 calc R . .
C15 C 0.1996(2) 0.7999(3) -0.0178(2) 0.0693(9) Uani 1 1 d . . .
H15 H 0.1282 0.7723 -0.0053 0.083 Uiso 1 1 calc R . .
C16 C 0.8490(3) 0.2279(2) 0.24117(15) 0.0519(6) Uani 1 1 d . . .
C17 C 0.7644(3) 0.1520(3) 0.2781(2) 0.0840(11) Uani 1 1 d . . .
H17A H 0.7756 0.0805 0.2574 0.126 Uiso 1 1 calc R . .
H17B H 0.6860 0.1749 0.2612 0.126 Uiso 1 1 calc R . .
H17C H 0.7777 0.1526 0.3390 0.126 Uiso 1 1 calc 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'
Zn Zn 0.2839 1.4301 '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
C12 Fe1 C10 86.47(9) . . ?
C12 Fe1 C11 89.27(9) . . ?
C10 Fe1 C11 87.79(9) . . ?
C12 Fe1 N3 92.10(8) . . ?
C10 Fe1 N3 176.71(8) . . ?
C11 Fe1 N3 89.23(8) . . ?
C12 Fe1 N5 92.05(8) . . ?
C10 Fe1 N5 93.86(8) . . ?
C11 Fe1 N5 177.94(8) . . ?
N3 Fe1 N5 89.14(7) . . ?
C12 Fe1 N1 179.25(8) . . ?
C10 Fe1 N1 92.79(8) . . ?
C11 Fe1 N1 90.73(8) . . ?
N3 Fe1 N1 88.65(7) . . ?
N5 Fe1 N1 87.96(7) . . ?
O2 Zn1 O1 102.97(8) . . ?
O2 Zn1 N9 130.56(8) . . ?
O1 Zn1 N9 109.48(9) . . ?
O2 Zn1 N7 105.82(8) . . ?
O1 Zn1 N7 101.88(8) . . ?
N9 Zn1 N7 102.82(8) . . ?
N10 B1 N2 114.04(17) . . ?
N10 B1 N6 113.34(17) . . ?
N2 B1 N6 105.86(15) . . ?
N10 B1 N4 108.61(16) . . ?
N2 B1 N4 107.52(16) . . ?
N6 B1 N4 107.12(16) . . ?
C1 N1 N2 107.15(16) . . ?
C1 N1 Fe1 131.64(15) . . ?
N2 N1 Fe1 120.95(12) . . ?
C3 N2 N1 108.54(16) . . ?
C3 N2 B1 134.16(18) . . ?
N1 N2 B1 116.99(15) . . ?
C4 N3 N4 107.30(16) . . ?
C4 N3 Fe1 134.14(15) . . ?
N4 N3 Fe1 118.52(12) . . ?
C6 N4 N3 109.12(17) . . ?
C6 N4 B1 130.57(18) . . ?
N3 N4 B1 120.31(15) . . ?
C7 N5 N6 106.48(16) . . ?
C7 N5 Fe1 132.49(14) . . ?
N6 N5 Fe1 120.84(12) . . ?
C9 N6 N5 109.25(15) . . ?
C9 N6 B1 133.71(17) . . ?
N5 N6 B1 117.00(15) . . ?
C12 N7 Zn1 172.39(19) . . ?
C10 N9 Zn1 170.7(2) 3_765 . ?
C13 N10 N11 110.1(2) . . ?
C13 N10 B1 127.8(2) . . ?
N11 N10 B1 118.89(18) . . ?
C15 N11 N10 105.5(2) . . ?
C16 O2 Zn1 111.37(17) . . ?
N1 C1 C2 110.1(2) . . ?
N1 C1 H1 124.9 . . ?
C2 C1 H1 124.9 . . ?
C3 C2 C1 105.37(19) . . ?
C3 C2 H2 127.3 . . ?
C1 C2 H2 127.3 . . ?
N2 C3 C2 108.78(19) . . ?
N2 C3 H3 125.6 . . ?
C2 C3 H3 125.6 . . ?
N3 C4 C5 109.9(2) . . ?
N3 C4 H4 125.1 . . ?
C5 C4 H4 125.1 . . ?
C6 C5 C4 105.41(19) . . ?
C6 C5 H5 127.3 . . ?
C4 C5 H5 127.3 . . ?
N4 C6 C5 108.3(2) . . ?
N4 C6 H6 125.8 . . ?
C5 C6 H6 125.8 . . ?
N5 C7 C8 110.48(18) . . ?
N5 C7 H7 124.8 . . ?
C8 C7 H7 124.8 . . ?
C7 C8 C9 105.18(18) . . ?
C7 C8 H8 127.4 . . ?
C9 C8 H8 127.4 . . ?
N6 C9 C8 108.59(18) . . ?
N6 C9 H9 125.7 . . ?
C8 C9 H9 125.7 . . ?
N9 C10 Fe1 177.2(2) 3_765 . ?
N8 C11 Fe1 175.0(2) . . ?
N7 C12 Fe1 179.4(2) . . ?
N10 C13 C14 106.2(3) . . ?
N10 C13 H13 126.9 . . ?
C14 C13 H13 126.9 . . ?
C15 C14 C13 106.9(2) . . ?
C15 C14 H14 126.6 . . ?
C13 C14 H14 126.6 . . ?
N11 C15 C14 111.2(3) . . ?
N11 C15 H15 124.4 . . ?
C14 C15 H15 124.4 . . ?
O3 C16 O2 122.4(2) . . ?
O3 C16 C17 120.9(3) . . ?
O2 C16 C17 116.6(3) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 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 C12 1.916(2) . ?
Fe1 C10 1.920(2) . ?
Fe1 C11 1.925(2) . ?
Fe1 N3 1.9536(16) . ?
Fe1 N5 1.9661(16) . ?
Fe1 N1 1.9702(16) . ?
Zn1 O2 1.9239(18) . ?
Zn1 O1 1.9659(18) . ?
Zn1 N9 1.9725(18) . ?
Zn1 N7 1.9955(18) . ?
B1 N10 1.500(3) . ?
B1 N2 1.547(3) . ?
B1 N6 1.551(3) . ?
B1 N4 1.553(3) . ?
N1 C1 1.334(2) . ?
N1 N2 1.363(2) . ?
N2 C3 1.353(3) . ?
N3 C4 1.336(3) . ?
N3 N4 1.354(2) . ?
N4 C6 1.347(2) . ?
N5 C7 1.339(3) . ?
N5 N6 1.365(2) . ?
N6 C9 1.340(3) . ?
N7 C12 1.139(3) . ?
N8 C11 1.143(3) . ?
N9 C10 1.140(3) 3_765 ?
N10 C13 1.363(3) . ?
N10 N11 1.373(3) . ?
N11 C15 1.324(3) . ?
O2 C16 1.270(3) . ?
O3 C16 1.230(3) . ?
C1 C2 1.382(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.367(3) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 C5 1.380(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.376(3) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.374(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.378(3) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 N9 1.140(3) 3_765 ?
C13 C14 1.371(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.364(5) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.513(4) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
