#------------------------------------------------------------------------------
#$Date: 2019-03-01 11:51:38 +0200 (Fri, 01 Mar 2019) $
#$Revision: 213925 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/01/45/2014597.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_2014597
loop_
_publ_author_name
'Yun-Ling, Gao'
'Xiao-Jun, Peng'
'Shi-Guo, Sun'
'Chang-Neng, Chen '
'Li-Cheng, Sun'
_publ_section_title
;μ-Oxo-bis{[(6-hydroxymethyl-2-pyridylmethyl)bis(2-pyridylmethyl)amine-κ⁵N,N',N'',N''',O]iron(III)}
 tetrakis(perchlorate)
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m13
_journal_page_last               m15
_journal_paper_doi               10.1107/S0108270104028148
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Fe2 O (C19 H20 N4 O)2] (Cl O4)4'
_chemical_formula_moiety         'C38 H40 Fe2 N8 O3 4+, 4Cl O4 -'
_chemical_formula_sum            'C38 H40 Cl4 Fe2 N8 O19'
_chemical_formula_weight         1166.28
_chemical_name_systematic
;
μ-Oxo-bis{[(6-hydroxymethyl-2-pyridylmethyl)bis(2-pyridylmethyl)amine
-κ⁵N,N',N'',N''',O]iron(III)} tetrakis(perchlorate)
;
_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                 111.220(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.0733(9)
_cell_length_b                   9.9223(3)
_cell_length_c                   20.5055(8)
_cell_measurement_reflns_used    3348
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      1.81
_cell_volume                     4565.9(3)
_computing_cell_refinement       'SMART and SAINT (Siemens,1994)'
_computing_data_collection       'SMART (Siemens,1996)'
_computing_data_reduction        'SAINT? and XPREP in SHELXTL (Siemens, 1994)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω 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  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0549
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7191
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.957
_exptl_absorpt_correction_T_max  .856
_exptl_absorpt_correction_T_min  .7128
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          .34
_exptl_crystal_size_mid          .28
_exptl_crystal_size_min          .16
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.475
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         4002
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_gt           0.0752
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0536P)²+58.9568P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1659
_refine_ls_wR_factor_ref         0.1910
_reflns_number_gt                3000
_reflns_number_total             4002
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            av1198.cif
_cod_data_source_block           I
_cod_depositor_comments
;
  Moved the _audit_creation_method data item out of the loop.

  Antanas Vaitkus,
  2019-03-01
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2014597
_cod_database_fobs_code          2014597
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_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
_atom_site_type_symbol
Fe1 0.29296(4) 0.79664(9) 0.08823(5) 0.0304(3) Uani d . 1 . . Fe
O1 0.3169(2) 0.6180(5) 0.1415(3) 0.0451(12) Uani d D 1 . . O
O2 0.2500 0.7500 0.0000 0.0445(17) Uani d S 1 . . O
O3 0.4608(4) 0.3527(12) 0.0495(4) 0.144(4) Uani d . 1 . . O
O4 0.4874(4) 0.4481(9) 0.1561(5) 0.119(3) Uani d . 1 . . O
O5 0.4691(4) 0.2171(8) 0.1403(5) 0.130(3) Uani d . 1 . . O
O6 0.3914(3) 0.3699(7) 0.1005(5) 0.102(3) Uani d . 1 . . O
O7 0.1601(3) 0.3947(9) 0.1270(4) 0.108(3) Uani d . 1 . . O
O8 0.2578(3) 0.3888(5) 0.1329(3) 0.0619(15) Uani d . 1 . . O
O9 0.2360(3) 0.4851(6) 0.2249(3) 0.0765(19) Uani d . 1 . . O
O10 0.2281(3) 0.2526(6) 0.2063(3) 0.0686(17) Uani d . 1 . . O
N1 0.2182(2) 0.8654(6) 0.1099(3) 0.0360(13) Uani d . 1 . . N
N2 0.2995(2) 1.0166(5) 0.0817(3) 0.0330(12) Uani d . 1 . . N
N3 0.3697(2) 0.8181(6) 0.0602(3) 0.0377(13) Uani d . 1 . . N
N4 0.3547(2) 0.8471(6) 0.1896(3) 0.0366(13) Uani d . 1 . . N
C1 0.1858(3) 0.7920(8) 0.1383(4) 0.0444(17) Uani d . 1 . . C
H1 0.1989 0.7062 0.1551 0.053 Uiso calc R 1 . . H
C2 0.1338(3) 0.8394(9) 0.1435(4) 0.057(2) Uani d . 1 . . C
H2 0.1122 0.7870 0.1636 0.068 Uiso calc R 1 . . H
C3 0.1144(3) 0.9659(10) 0.1180(4) 0.062(2) Uani d . 1 . . C
H3 0.0789 0.9989 0.1199 0.074 Uiso calc R 1 . . H
C4 0.1473(3) 1.0440(8) 0.0899(4) 0.051(2) Uani d . 1 . . C
H4 0.1350 1.1307 0.0739 0.062 Uiso calc R 1 . . H
C5 0.1996(3) 0.9903(7) 0.0859(3) 0.0402(16) Uani d . 1 . . C
C6 0.2364(3) 1.0635(7) 0.0511(4) 0.0420(16) Uani d . 1 . . C
H6A 0.2206 1.0458 0.0012 0.050 Uiso calc R 1 . . H
H6B 0.2346 1.1598 0.0581 0.050 Uiso calc R 1 . . H
C7 0.3320(3) 1.0455(7) 0.0336(4) 0.0440(17) Uani d . 1 . . C
H7A 0.3528 1.1308 0.0467 0.053 Uiso calc R 1 . . H
H7B 0.3034 1.0544 -0.0137 0.053 Uiso calc R 1 . . H
C8 0.3762(3) 0.9382(7) 0.0349(3) 0.0394(16) Uani d . 1 . . C
C9 0.4190(3) 0.9582(8) 0.0047(4) 0.0502(19) Uani d . 1 . . C
H9 0.4233 1.0419 -0.0133 0.060 Uiso calc R 1 . . H
C10 0.4547(3) 0.8514(9) 0.0020(5) 0.060(2) Uani d . 1 . . C
H10 0.4831 0.8620 -0.0186 0.072 Uiso calc R 1 . . H
C11 0.4482(3) 0.7299(8) 0.0297(4) 0.0490(19) Uani d . 1 . . C
H11 0.4727 0.6579 0.0289 0.059 Uiso calc R 1 . . H
C12 0.4057(3) 0.7147(7) 0.0586(4) 0.0428(16) Uani d . 1 . . C
H12 0.4014 0.6319 0.0775 0.051 Uiso calc R 1 . . H
C13 0.3296(3) 1.0761(7) 0.1530(3) 0.0401(16) Uani d . 1 . . C
H13A 0.3514 1.1562 0.1494 0.048 Uiso calc R 1 . . H
H13B 0.2997 1.1027 0.1720 0.048 Uiso calc R 1 . . H
C14 0.3716(3) 0.9777(7) 0.2016(3) 0.0344(14) Uani d . 1 . . C
C15 0.4222(3) 1.0126(8) 0.2575(4) 0.0476(18) Uani d . 1 . . C
H15 0.4340 1.1022 0.2659 0.057 Uiso calc R 1 . . H
C16 0.4549(4) 0.9118(9) 0.3004(4) 0.059(2) Uani d . 1 . . C
H16 0.4889 0.9337 0.3384 0.071 Uiso calc R 1 . . H
C17 0.4379(3) 0.7788(8) 0.2880(4) 0.052(2) Uani d . 1 . . C
H17 0.4600 0.7106 0.3170 0.063 Uiso calc R 1 . . H
C18 0.3866(3) 0.7498(7) 0.2306(3) 0.0399(16) Uani d . 1 . . C
C19 0.3628(3) 0.6109(7) 0.2110(4) 0.0505(19) Uani d . 1 . . C
H19A 0.3945 0.5506 0.2108 0.061 Uiso calc R 1 . . H
H19B 0.3461 0.5771 0.2444 0.061 Uiso calc R 1 . . H
Cl1 0.45259(9) 0.3448(2) 0.11403(12) 0.0582(5) Uani d . 1 . . Cl
Cl2 0.21960(9) 0.38082(18) 0.17381(10) 0.0492(5) Uani d . 1 . . Cl
H20 0.297(3) 0.546(5) 0.133(4) 0.07(3) Uiso d D 1 . . H
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'
Cl Cl 0.1484 0.1585 '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_3
_geom_angle
_geom_angle_publ_flag
O2 Fe1 O1 . 105.26(15) yes
O2 Fe1 N1 . 94.12(14) yes
O1 Fe1 N1 . 105.2(2) yes
O2 Fe1 N4 . 172.06(15) yes
O1 Fe1 N4 . 73.8(2) yes
N1 Fe1 N4 . 93.7(2) yes
O2 Fe1 N3 . 89.61(14) yes
O1 Fe1 N3 . 97.2(2) yes
N1 Fe1 N3 . 155.3(2) yes
N4 Fe1 N3 . 82.7(2) yes
O2 Fe1 N2 . 102.90(14) yes
O1 Fe1 N2 . 151.4(2) yes
N1 Fe1 N2 . 77.1(2) yes
N4 Fe1 N2 . 77.6(2) yes
N3 Fe1 N2 . 78.3(2) yes
C19 O1 Fe1 . 122.1(4) ?
C19 O1 H20 . 109(6) ?
Fe1 O1 H20 . 127(6) ?
Fe1 O2 Fe1 7_565 180.00(5) yes
C1 N1 C5 . 119.1(6) ?
C1 N1 Fe1 . 126.0(5) ?
C5 N1 Fe1 . 114.5(4) ?
C7 N2 C6 . 111.1(5) ?
C7 N2 C13 . 112.6(5) ?
C6 N2 C13 . 110.3(5) ?
C7 N2 Fe1 . 107.3(4) ?
C6 N2 Fe1 . 104.5(4) ?
C13 N2 Fe1 . 110.6(4) ?
C8 N3 C12 . 120.2(6) ?
C8 N3 Fe1 . 115.5(4) ?
C12 N3 Fe1 . 123.8(5) ?
C18 N4 C14 . 120.9(6) ?
C18 N4 Fe1 . 119.1(5) ?
C14 N4 Fe1 . 117.4(4) ?
N1 C1 C2 . 122.4(7) ?
N1 C1 H1 . 118.8 ?
C2 C1 H1 . 118.8 ?
C3 C2 C1 . 118.4(8) ?
C3 C2 H2 . 120.8 ?
C1 C2 H2 . 120.8 ?
C4 C3 C2 . 120.5(7) ?
C4 C3 H3 . 119.8 ?
C2 C3 H3 . 119.8 ?
C3 C4 C5 . 118.6(7) ?
C3 C4 H4 . 120.7 ?
C5 C4 H4 . 120.7 ?
N1 C5 C4 . 121.1(7) ?
N1 C5 C6 . 116.1(6) ?
C4 C5 C6 . 122.7(7) ?
N2 C6 C5 . 109.5(5) ?
N2 C6 H6A . 109.8 ?
C5 C6 H6A . 109.8 ?
N2 C6 H6B . 109.8 ?
C5 C6 H6B . 109.8 ?
H6A C6 H6B . 108.2 ?
N2 C7 C8 . 113.0(5) ?
N2 C7 H7A . 109.0 ?
C8 C7 H7A . 109.0 ?
N2 C7 H7B . 109.0 ?
C8 C7 H7B . 109.0 ?
H7A C7 H7B . 107.8 ?
N3 C8 C9 . 120.7(7) ?
N3 C8 C7 . 117.4(6) ?
C9 C8 C7 . 121.6(6) ?
C10 C9 C8 . 118.6(7) ?
C10 C9 H9 . 120.7 ?
C8 C9 H9 . 120.7 ?
C11 C10 C9 . 119.7(7) ?
C11 C10 H10 . 120.1 ?
C9 C10 H10 . 120.1 ?
C12 C11 C10 . 119.7(7) ?
C12 C11 H11 . 120.2 ?
C10 C11 H11 . 120.2 ?
N3 C12 C11 . 121.1(7) ?
N3 C12 H12 . 119.5 ?
C11 C12 H12 . 119.5 ?
C14 C13 N2 . 111.4(5) ?
C14 C13 H13A . 109.3 ?
N2 C13 H13A . 109.3 ?
C14 C13 H13B . 109.3 ?
N2 C13 H13B . 109.3 ?
H13A C13 H13B . 108.0 ?
N4 C14 C15 . 120.5(6) ?
N4 C14 C13 . 114.6(5) ?
C15 C14 C13 . 124.8(6) ?
C16 C15 C14 . 118.5(7) ?
C16 C15 H15 . 120.8 ?
C14 C15 H15 . 120.8 ?
C15 C16 C17 . 121.1(7) ?
C15 C16 H16 . 119.5 ?
C17 C16 H16 . 119.5 ?
C16 C17 C18 . 117.8(7) ?
C16 C17 H17 . 121.1 ?
C18 C17 H17 . 121.1 ?
N4 C18 C17 . 121.2(7) ?
N4 C18 C19 . 115.1(6) ?
C17 C18 C19 . 123.7(7) ?
O1 C19 C18 . 107.5(6) ?
O1 C19 H19A . 110.2 ?
C18 C19 H19A . 110.2 ?
O1 C19 H19B . 110.2 ?
C18 C19 H19B . 110.2 ?
H19A C19 H19B . 108.5 ?
O5 Cl1 O4 . 114.0(6) ?
O5 Cl1 O3 . 107.5(7) ?
O4 Cl1 O3 . 106.3(6) ?
O5 Cl1 O6 . 111.7(5) ?
O4 Cl1 O6 . 109.8(5) ?
O3 Cl1 O6 . 107.2(5) ?
O7 Cl2 O10 . 110.2(5) ?
O7 Cl2 O9 . 111.9(5) ?
O10 Cl2 O9 . 110.7(4) ?
O7 Cl2 O8 . 107.5(4) ?
O10 Cl2 O8 . 107.9(4) ?
O9 Cl2 O8 . 108.7(4) ?
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 O2 . 1.7896(9) yes
Fe1 O1 . 2.052(5) yes
Fe1 N1 . 2.117(5) yes
Fe1 N4 . 2.132(5) yes
Fe1 N3 . 2.134(5) yes
Fe1 N2 . 2.196(5) yes
O1 C19 . 1.455(9) ?
O1 H20 . 0.84(6) ?
O2 Fe1 7_565 1.7896(9) ?
O3 Cl1 . 1.409(8) ?
O4 Cl1 . 1.404(8) ?
O5 Cl1 . 1.378(7) ?
O6 Cl1 . 1.418(6) ?
O7 Cl2 . 1.413(7) ?
O8 Cl2 . 1.454(5) ?
O9 Cl2 . 1.423(6) ?
O10 Cl2 . 1.415(6) ?
N1 C1 . 1.346(9) ?
N1 C5 . 1.349(9) ?
N2 C7 . 1.492(8) ?
N2 C6 . 1.492(8) ?
N2 C13 . 1.499(8) ?
N3 C8 . 1.332(8) ?
N3 C12 . 1.351(8) ?
N4 C18 . 1.328(8) ?
N4 C14 . 1.354(8) ?
C1 C2 . 1.376(10) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.374(12) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.374(11) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.396(9) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.510(10) ?
C6 H6A . 0.9700 ?
C6 H6B . 0.9700 ?
C7 C8 . 1.498(9) ?
C7 H7A . 0.9700 ?
C7 H7B . 0.9700 ?
C8 C9 . 1.395(9) ?
C9 C10 . 1.378(11) ?
C9 H9 . 0.9300 ?
C10 C11 . 1.365(11) ?
C10 H10 . 0.9300 ?
C11 C12 . 1.363(10) ?
C11 H11 . 0.9300 ?
C12 H12 . 0.9300 ?
C13 C14 . 1.496(9) ?
C13 H13A . 0.9700 ?
C13 H13B . 0.9700 ?
C14 C15 . 1.379(9) ?
C15 C16 . 1.376(11) ?
C15 H15 . 0.9300 ?
C16 C17 . 1.377(11) ?
C16 H16 . 0.9300 ?
C17 C18 . 1.393(10) ?
C17 H17 . 0.9300 ?
C18 C19 . 1.491(10) ?
C19 H19A . 0.9700 ?
C19 H19B . 0.9700 ?
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
O1 H20 O8 0.84(6) 1.82(3) 2.654(7) 169(8)
