#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/10/2221090.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# 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_2221090
loop_
_publ_author_name
'Liu, Qingyun'
'Pan, Shuying'
'Wang, Dongmei'
_publ_section_title
;Di-μ-hydroxido-bis({2,2'-[propane-1,3-diylbis(nitrilomethylidyne)]diphenolato}iron(III))
 dimethylformamide disolvate
;
_journal_coeditor_code           HG2478
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m305
_journal_paper_doi               10.1107/S1600536809005091
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Fe2 (C17 H16 N2 O2)2 (O H)2], 2C3 H7 N'
_chemical_formula_moiety         'C34 H34 Fe2 N4 O6, 2(C3 H7 N O)'
_chemical_formula_sum            'C40 H48 Fe2 N6 O8'
_chemical_formula_weight         852.54
_chemical_name_systematic
;Di-μ-hydroxido-bis({2,2'-[propane-1,3-
diylbis(nitrilomethylidyne)]diphenolato}iron(III))
 dimethylformamide disolvate
;
_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                 101.27(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.768(2)
_cell_length_b                   10.136(2)
_cell_length_c                   17.540(4)
_cell_measurement_reflns_used    221
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      3.11
_cell_volume                     1877.5(7)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'XP in SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10664
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    0.836
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_correction_T_min  0.862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.651
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0464
_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)+(0.0957P)²+1.7319P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1370
_refine_ls_wR_factor_ref         0.1425
_reflns_number_gt                2809
_reflns_number_total             3221
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hg2478.cif
_cod_data_source_block           I
_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 

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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2221090
_cod_database_fobs_code          2221090
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_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe1 0.50501(4) 0.37734(4) 0.03284(2) 0.01386(19) Uani d . 1 . .
O O1 0.54651(17) 0.43569(19) 0.13793(11) 0.0140(4) Uani d . 1 . .
O O2 0.63819(18) 0.24760(19) 0.05879(11) 0.0148(4) Uani d . 1 . .
O O3 0.39002(17) 0.50795(18) 0.00288(10) 0.0127(4) Uani d . 1 . .
H H3B 0.3390 0.5576 0.0209 0.015 Uiso d R 1 . .
O O4 0.9440(2) 0.6587(3) 0.27864(14) 0.0360(6) Uani d . 1 . .
N N1 0.3654(2) 0.2624(2) 0.06536(13) 0.0135(5) Uani d . 1 . .
N N2 0.4579(2) 0.2834(2) -0.07001(13) 0.0128(5) Uani d . 1 . .
N N3 0.9331(2) 0.5320(3) 0.16973(15) 0.0251(6) Uani d . 1 . .
C C1 0.4628(3) 0.4666(3) 0.18093(15) 0.0131(6) Uani d . 1 . .
C C2 0.4952(3) 0.5623(3) 0.24001(17) 0.0186(6) Uani d . 1 . .
H H2A 0.5754 0.6002 0.2486 0.022 Uiso calc R 1 . .
C C3 0.4098(3) 0.6008(3) 0.28532(18) 0.0216(7) Uani d . 1 . .
H H3A 0.4322 0.6665 0.3225 0.026 Uiso calc R 1 . .
C C4 0.2905(3) 0.5423(3) 0.27608(17) 0.0213(7) Uani d . 1 . .
H H4A 0.2329 0.5701 0.3059 0.026 Uiso calc R 1 . .
C C5 0.2586(3) 0.4420(3) 0.22176(17) 0.0206(7) Uani d . 1 . .
H H5A 0.1811 0.3993 0.2173 0.025 Uiso calc R 1 . .
C C6 0.3431(3) 0.4043(3) 0.17312(17) 0.0152(6) Uani d . 1 . .
C C7 0.3077(3) 0.2952(3) 0.12009(16) 0.0156(6) Uani d . 1 . .
H H7A 0.2379 0.2451 0.1261 0.019 Uiso calc R 1 . .
C C8 0.3228(3) 0.1439(3) 0.01922(18) 0.0190(6) Uani d . 1 . .
H H8A 0.2676 0.0928 0.0454 0.023 Uiso calc R 1 . .
H H8B 0.3957 0.0897 0.0156 0.023 Uiso calc R 1 . .
C C9 0.2526(3) 0.1786(3) -0.06223(17) 0.0231(7) Uani d . 1 . .
H H9A 0.1701 0.2139 -0.0589 0.028 Uiso calc R 1 . .
H H9B 0.2391 0.0985 -0.0930 0.028 Uiso calc R 1 . .
C C10 0.3225(3) 0.2798(3) -0.10456(17) 0.0170(6) Uani d . 1 . .
H H10A 0.3116 0.2562 -0.1591 0.020 Uiso calc R 1 . .
H H10B 0.2861 0.3666 -0.1013 0.020 Uiso calc R 1 . .
C C11 0.5369(3) 0.2250(3) -0.10447(16) 0.0146(6) Uani d . 1 . .
H H11A 0.5069 0.1928 -0.1543 0.018 Uiso calc R 1 . .
C C12 0.6696(3) 0.2055(3) -0.07143(17) 0.0149(6) Uani d . 1 . .
C C13 0.7523(3) 0.1622(3) -0.11903(18) 0.0199(6) Uani d . 1 . .
H H13A 0.7222 0.1542 -0.1723 0.024 Uiso calc R 1 . .
C C14 0.8760(3) 0.1314(3) -0.0891(2) 0.0236(7) Uani d . 1 . .
H H14A 0.9297 0.1035 -0.1215 0.028 Uiso calc R 1 . .
C C15 0.9204(3) 0.1426(3) -0.00837(19) 0.0209(7) Uani d . 1 . .
H H15A 1.0046 0.1232 0.0124 0.025 Uiso calc R 1 . .
C C16 0.8409(3) 0.1821(3) 0.04073(17) 0.0172(6) Uani d . 1 . .
H H16A 0.8718 0.1870 0.0940 0.021 Uiso calc R 1 . .
C C17 0.7135(3) 0.2150(3) 0.01030(17) 0.0146(6) Uani d . 1 . .
C C18 0.9718(3) 0.6354(3) 0.2146(2) 0.0293(8) Uani d . 1 . .
H H18A 1.0243 0.6957 0.1964 0.035 Uiso calc R 1 . .
C C19 0.8528(3) 0.4313(3) 0.1945(2) 0.0289(7) Uani d . 1 . .
H H19A 0.8366 0.4537 0.2448 0.043 Uiso calc R 1 . .
H H19B 0.8948 0.3474 0.1971 0.043 Uiso calc R 1 . .
H H19C 0.7741 0.4264 0.1578 0.043 Uiso calc R 1 . .
C C20 0.9676(4) 0.5132(4) 0.0947(2) 0.0354(8) Uani d . 1 . .
H H20A 1.0208 0.5846 0.0847 0.053 Uiso calc R 1 . .
H H20B 0.8924 0.5111 0.0549 0.053 Uiso calc R 1 . .
H H20C 1.0125 0.4314 0.0946 0.053 Uiso calc R 1 . .
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'
K K 0.2009 0.2494 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O3 Fe1 O3 3_665 . 82.46(9) ?
O3 Fe1 O1 3_665 . 95.22(8) ?
O3 Fe1 O1 . . 94.09(8) ?
O3 Fe1 O2 3_665 . 91.93(8) ?
O3 Fe1 O2 . . 174.23(8) ?
O1 Fe1 O2 . . 87.73(9) ?
O3 Fe1 N2 3_665 . 93.36(9) ?
O3 Fe1 N2 . . 92.70(9) ?
O1 Fe1 N2 . . 169.68(9) ?
O2 Fe1 N2 . . 86.26(9) ?
O3 Fe1 N1 3_665 . 172.13(9) ?
O3 Fe1 N1 . . 89.95(9) ?
O1 Fe1 N1 . . 87.35(9) ?
O2 Fe1 N1 . . 95.61(9) ?
N2 Fe1 N1 . . 84.90(9) ?
O3 Fe1 Fe1 3_665 3_665 41.26(6) ?
O3 Fe1 Fe1 . 3_665 41.20(6) ?
O1 Fe1 Fe1 . 3_665 96.19(6) ?
O2 Fe1 Fe1 . 3_665 133.18(6) ?
N2 Fe1 Fe1 . 3_665 94.03(7) ?
N1 Fe1 Fe1 . 3_665 131.11(7) ?
C1 O1 Fe1 . . 124.69(17) ?
C17 O2 Fe1 . . 122.47(17) ?
Fe1 O3 Fe1 3_665 . 97.54(9) ?
Fe1 O3 H3B 3_665 . 103.9 ?
Fe1 O3 H3B . . 140.9 ?
C7 N1 C8 . . 118.6(2) ?
C7 N1 Fe1 . . 122.95(19) ?
C8 N1 Fe1 . . 118.25(17) ?
C11 N2 C10 . . 119.5(2) ?
C11 N2 Fe1 . . 124.5(2) ?
C10 N2 Fe1 . . 115.99(17) ?
C18 N3 C20 . . 122.4(3) ?
C18 N3 C19 . . 120.8(3) ?
C20 N3 C19 . . 116.8(3) ?
O1 C1 C2 . . 118.9(2) ?
O1 C1 C6 . . 123.2(3) ?
C2 C1 C6 . . 117.8(2) ?
C3 C2 C1 . . 121.2(3) ?
C3 C2 H2A . . 119.4 ?
C1 C2 H2A . . 119.4 ?
C2 C3 C4 . . 120.9(3) ?
C2 C3 H3A . . 119.5 ?
C4 C3 H3A . . 119.5 ?
C3 C4 C5 . . 119.2(3) ?
C3 C4 H4A . . 120.4 ?
C5 C4 H4A . . 120.4 ?
C4 C5 C6 . . 120.6(3) ?
C4 C5 H5A . . 119.7 ?
C6 C5 H5A . . 119.7 ?
C1 C6 C5 . . 120.0(3) ?
C1 C6 C7 . . 121.6(2) ?
C5 C6 C7 . . 118.3(3) ?
N1 C7 C6 . . 124.9(3) ?
N1 C7 H7A . . 117.5 ?
C6 C7 H7A . . 117.5 ?
N1 C8 C9 . . 111.9(2) ?
N1 C8 H8A . . 109.2 ?
C9 C8 H8A . . 109.2 ?
N1 C8 H8B . . 109.2 ?
C9 C8 H8B . . 109.2 ?
H8A C8 H8B . . 107.9 ?
C8 C9 C10 . . 113.9(2) ?
C8 C9 H9A . . 108.8 ?
C10 C9 H9A . . 108.8 ?
C8 C9 H9B . . 108.8 ?
C10 C9 H9B . . 108.8 ?
H9A C9 H9B . . 107.7 ?
N2 C10 C9 . . 110.9(2) ?
N2 C10 H10A . . 109.5 ?
C9 C10 H10A . . 109.5 ?
N2 C10 H10B . . 109.5 ?
C9 C10 H10B . . 109.5 ?
H10A C10 H10B . . 108.0 ?
N2 C11 C12 . . 124.7(3) ?
N2 C11 H11A . . 117.6 ?
C12 C11 H11A . . 117.6 ?
C13 C12 C17 . . 119.7(3) ?
C13 C12 C11 . . 119.7(3) ?
C17 C12 C11 . . 120.1(2) ?
C14 C13 C12 . . 121.7(3) ?
C14 C13 H13A . . 119.2 ?
C12 C13 H13A . . 119.2 ?
C13 C14 C15 . . 118.8(3) ?
C13 C14 H14A . . 120.6 ?
C15 C14 H14A . . 120.6 ?
C16 C15 C14 . . 121.2(3) ?
C16 C15 H15A . . 119.4 ?
C14 C15 H15A . . 119.4 ?
C15 C16 C17 . . 120.4(3) ?
C15 C16 H16A . . 119.8 ?
C17 C16 H16A . . 119.8 ?
O2 C17 C16 . . 119.2(3) ?
O2 C17 C12 . . 122.6(2) ?
C16 C17 C12 . . 118.2(2) ?
O4 C18 N3 . . 125.7(3) ?
O4 C18 H18A . . 117.1 ?
N3 C18 H18A . . 117.1 ?
N3 C19 H19A . . 109.5 ?
N3 C19 H19B . . 109.5 ?
H19A C19 H19B . . 109.5 ?
N3 C19 H19C . . 109.5 ?
H19A C19 H19C . . 109.5 ?
H19B C19 H19C . . 109.5 ?
N3 C20 H20A . . 109.5 ?
N3 C20 H20B . . 109.5 ?
H20A C20 H20B . . 109.5 ?
N3 C20 H20C . . 109.5 ?
H20A C20 H20C . . 109.5 ?
H20B C20 H20C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 O3 3_665 1.8163(18) ?
Fe1 O3 . 1.8186(19) ?
Fe1 O1 . 1.9040(19) ?
Fe1 O2 . 1.9334(19) ?
Fe1 N2 . 2.015(2) ?
Fe1 N1 . 2.069(2) ?
Fe1 Fe1 3_665 2.7337(9) ?
O1 C1 . 1.321(3) ?
O2 C17 . 1.327(3) ?
O3 Fe1 3_665 1.8163(18) ?
O3 H3B . 0.8500 ?
O4 C18 . 1.241(4) ?
N1 C7 . 1.285(4) ?
N1 C8 . 1.471(4) ?
N2 C11 . 1.281(4) ?
N2 C10 . 1.465(4) ?
N3 C18 . 1.328(4) ?
N3 C20 . 1.449(4) ?
N3 C19 . 1.458(4) ?
C1 C2 . 1.412(4) ?
C1 C6 . 1.417(4) ?
C2 C3 . 1.384(4) ?
C2 H2A . 0.9300 ?
C3 C4 . 1.395(5) ?
C3 H3A . 0.9300 ?
C4 C5 . 1.389(4) ?
C4 H4A . 0.9300 ?
C5 C6 . 1.416(4) ?
C5 H5A . 0.9300 ?
C6 C7 . 1.447(4) ?
C7 H7A . 0.9300 ?
C8 C9 . 1.521(4) ?
C8 H8A . 0.9700 ?
C8 H8B . 0.9700 ?
C9 C10 . 1.546(4) ?
C9 H9A . 0.9700 ?
C9 H9B . 0.9700 ?
C10 H10A . 0.9700 ?
C10 H10B . 0.9700 ?
C11 C12 . 1.447(4) ?
C11 H11A . 0.9300 ?
C12 C13 . 1.405(4) ?
C12 C17 . 1.422(4) ?
C13 C14 . 1.369(4) ?
C13 H13A . 0.9300 ?
C14 C15 . 1.407(5) ?
C14 H14A . 0.9300 ?
C15 C16 . 1.386(4) ?
C15 H15A . 0.9300 ?
C16 C17 . 1.412(4) ?
C16 H16A . 0.9300 ?
C18 H18A . 0.9300 ?
C19 H19A . 0.9600 ?
C19 H19B . 0.9600 ?
C19 H19C . 0.9600 ?
C20 H20A . 0.9600 ?
C20 H20B . 0.9600 ?
C20 H20C . 0.9600 ?
