#------------------------------------------------------------------------------
#$Date: 2019-11-25 02:45:19 +0200 (Mon, 25 Nov 2019) $
#$Revision: 239979 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/35/06/4350661.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_4350661
loop_
_publ_author_name
'Anwar, Muhammad U.'
'Dawe, Louise N.'
'Parsons, Stewart R.'
'Tandon, Santokh S.'
'Thompson, Laurence K.'
'Dey, Subrata K.'
'Mereacre, Valeriu'
'Reiff, William M.'
'Bunge, Scott D.'
_publ_section_title
;
 Oligonuclear Fe complexes (Fe, Fe4, Fe6, Fe9) derived from tritopic
 pyridine bis-hydrazone ligands-structural, magnetic, and Mössbauer
 studies.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4655
_journal_page_last               4668
_journal_paper_doi               10.1021/ic500348k
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C17 H19 Fe N12 O7, 2(N O3), 3(H2 O)'
_chemical_formula_sum            'C17 H25 Fe N14 O16'
_chemical_formula_weight         737.32
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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                 121.286(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.157(3)
_cell_length_b                   21.058(4)
_cell_length_c                   11.798(3)
_cell_measurement_reflns_used    6089
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      30.5866
_cell_measurement_theta_min      1.9414
_cell_volume                     3005.7(12)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_publication_material  'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  'graphite - Rigaku SHINE'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19492
_diffrn_reflns_theta_full        26.49
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    0.598
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8751
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'Light red'
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1516
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.936
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         3120
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0671
_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)+(0.1180P)²+4.6993P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1936
_refine_ls_wR_factor_ref         0.1946
_reflns_number_gt                3073
_reflns_number_total             3120
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500348k_si_002.cif
_cod_data_source_block           Complex_1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        3005.8(11)
_cod_database_code               4350661
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_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
Fe1 Fe 1.0000 0.19053(3) 0.2500 0.0339(2) Uani 1 2 d S
O1 O 0.95552(18) 0.21635(11) 0.3837(2) 0.0397(5) Uani 1 1 d .
O2 O 0.9776(2) 0.10061(12) 0.3232(3) 0.0629(8) Uani 1 1 d .
O3 O 1.0000 0.01049(19) 0.2500 0.101(2) Uani 1 2 d S
O4 O 0.6989(2) 0.12729(11) 0.1509(2) 0.0442(6) Uani 1 1 d .
O5 O 0.7380(3) 0.04989(14) 0.0629(3) 0.0659(8) Uani 1 1 d .
O6 O 0.6292(3) 0.03407(14) 0.1355(4) 0.0723(9) Uani 1 1 d .
O7 O 1.16071(18) 0.18856(10) 0.3948(2) 0.0379(5) Uani 1 1 d .
H9 H 1.2070 0.1711 0.3679 0.045 Uiso 1 1 d .
H10 H 1.1465 0.1746 0.4595 0.045 Uiso 1 1 d .
O8 O 0.9116(3) 0.44042(15) 0.5907(3) 0.0754(9) Uani 1 1 d .
O9 O 0.8627(9) 0.0431(5) 0.4549(11) 0.123(3) Uani 0.50 1 d P
N1 N 0.8506(3) 0.15604(15) 0.6550(3) 0.0505(7) Uani 1 1 d .
N2 N 0.8105(2) 0.17116(14) 0.8609(3) 0.0408(6) Uani 1 1 d .
N3 N 0.8638(2) 0.32587(14) 0.6661(3) 0.0401(6) Uani 1 1 d .
H4 H 0.8776 0.3566 0.6262 0.048 Uiso 1 1 calc R
H5 H 0.8454 0.3351 0.7249 0.048 Uiso 1 1 calc R
N4 N 0.8978(2) 0.25143(15) 0.5499(2) 0.0395(6) Uani 1 1 d .
H6 H 0.9012 0.2113 0.5314 0.047 Uiso 1 1 calc R
N5 N 0.9214(2) 0.29943(14) 0.4868(3) 0.0400(6) Uani 1 1 d .
N6 N 1.0000 0.29032(17) 0.2500 0.0295(7) Uani 1 2 d S
N7 N 1.0000 0.0675(2) 0.2500 0.0690(15) Uani 1 2 d S
N8 N 0.6889(2) 0.06930(14) 0.1165(3) 0.0452(7) Uani 1 1 d .
C1 C 0.8313(4) 0.10628(18) 0.7095(4) 0.0606(10) Uani 1 1 d .
H1 H 0.8306 0.0649 0.6771 0.073 Uiso 1 1 calc R
C2 C 0.8120(3) 0.11385(18) 0.8135(4) 0.0533(9) Uani 1 1 d .
H2 H 0.7996 0.0773 0.8514 0.064 Uiso 1 1 calc R
C3 C 0.8282(2) 0.22092(16) 0.8043(3) 0.0356(6) Uani 1 1 d .
H3 H 0.8272 0.2625 0.8348 0.043 Uiso 1 1 calc R
C4 C 0.8481(2) 0.21315(15) 0.7017(3) 0.0343(6) Uani 1 1 d .
C5 C 0.8704(2) 0.26669(16) 0.6380(3) 0.0360(7) Uani 1 1 d .
C6 C 0.9489(2) 0.27569(15) 0.4052(3) 0.0340(6) Uani 1 1 d .
C7 C 0.9746(2) 0.32122(15) 0.3292(3) 0.0337(6) Uani 1 1 d .
C8 C 0.9725(3) 0.38677(16) 0.3314(3) 0.0439(7) Uani 1 1 d .
H7 H 0.9529 0.4086 0.3867 0.053 Uiso 1 1 calc R
C9 C 1.0000 0.4200(2) 0.2500 0.0489(11) Uani 1 2 d S
H8 H 1.0000 0.4651 0.2500 0.059 Uiso 1 2 calc SR
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'
Fe Fe 0.3463 0.8444 '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'
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
O7 Fe1 O7 177.64(12) . 2_755
O7 Fe1 O1 90.89(9) . .
O7 Fe1 O1 89.74(9) 2_755 .
O7 Fe1 O1 89.73(9) . 2_755
O7 Fe1 O1 90.89(9) 2_755 2_755
O1 Fe1 O1 149.29(13) . 2_755
O7 Fe1 N6 91.18(6) . .
O7 Fe1 N6 91.18(6) 2_755 .
O1 Fe1 N6 74.64(7) . .
O1 Fe1 N6 74.64(7) 2_755 .
O7 Fe1 O2 88.78(10) . .
O7 Fe1 O2 89.17(10) 2_755 .
O1 Fe1 O2 76.03(11) . .
O1 Fe1 O2 134.68(11) 2_755 .
N6 Fe1 O2 150.67(9) . .
O7 Fe1 O2 89.17(10) . 2_755
O7 Fe1 O2 88.78(10) 2_755 2_755
O1 Fe1 O2 134.68(11) . 2_755
O1 Fe1 O2 76.03(11) 2_755 2_755
N6 Fe1 O2 150.67(9) . 2_755
O2 Fe1 O2 58.65(18) . 2_755
C6 O1 Fe1 119.40(18) . .
N7 O2 Fe1 93.9(3) . .
Fe1 O7 H9 113.6 . .
Fe1 O7 H10 94.1 . .
H9 O7 H10 129.6 . .
C1 N1 C4 117.1(3) . .
C3 N2 C2 116.9(3) . .
C5 N3 H4 120.0 . .
C5 N3 H5 120.0 . .
H4 N3 H5 120.0 . .
C5 N4 N5 119.5(3) . .
C5 N4 H6 120.2 . .
N5 N4 H6 120.2 . .
C6 N5 N4 111.1(3) . .
C7 N6 C7 121.5(4) 2_755 .
C7 N6 Fe1 119.23(19) 2_755 .
C7 N6 Fe1 119.23(19) . .
O3 N7 O2 123.3(2) . 2_755
O3 N7 O2 123.3(2) . .
O2 N7 O2 113.4(4) 2_755 .
O5 N8 O6 121.3(3) . .
O5 N8 O4 119.0(3) . .
O6 N8 O4 119.7(3) . .
N1 C1 C2 121.2(3) . .
N1 C1 H1 119.4 . .
C2 C1 H1 119.4 . .
N2 C2 C1 121.5(3) . .
N2 C2 H2 119.2 . .
C1 C2 H2 119.2 . .
N2 C3 C4 121.3(3) . .
N2 C3 H3 119.3 . .
C4 C3 H3 119.3 . .
N1 C4 C3 121.9(3) . .
N1 C4 C5 114.9(3) . .
C3 C4 C5 123.2(3) . .
N3 C5 N4 121.3(3) . .
N3 C5 C4 122.5(3) . .
N4 C5 C4 116.2(3) . .
O1 C6 N5 126.5(3) . .
O1 C6 C7 116.3(2) . .
N5 C6 C7 117.2(3) . .
N6 C7 C8 121.1(3) . .
N6 C7 C6 110.4(3) . .
C8 C7 C6 128.4(3) . .
C7 C8 C9 118.2(3) . .
C7 C8 H7 120.9 . .
C9 C8 H7 120.9 . .
C8 C9 C8 119.8(4) 2_755 .
C8 C9 H8 120.1 2_755 .
C8 C9 H8 120.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O7 2.015(2) .
Fe1 O7 2.015(2) 2_755
Fe1 O1 2.053(2) .
Fe1 O1 2.053(2) 2_755
Fe1 N6 2.101(4) .
Fe1 O2 2.172(3) .
Fe1 O2 2.172(3) 2_755
O1 C6 1.288(4) .
O2 N7 1.272(4) .
O3 N7 1.200(6) .
O4 N8 1.271(4) .
O5 N8 1.227(4) .
O6 N8 1.230(4) .
O7 H9 0.9388 .
O7 H10 0.9318 .
N1 C1 1.330(5) .
N1 C4 1.331(4) .
N2 C3 1.334(4) .
N2 C2 1.335(5) .
N3 C5 1.305(4) .
N3 H4 0.8800 .
N3 H5 0.8800 .
N4 C5 1.325(4) .
N4 N5 1.395(4) .
N4 H6 0.8800 .
N5 C6 1.310(4) .
N6 C7 1.332(3) 2_755
N6 C7 1.333(3) .
N7 O2 1.272(4) 2_755
C1 C2 1.398(6) .
C1 H1 0.9500 .
C2 H2 0.9500 .
C3 C4 1.387(4) .
C3 H3 0.9500 .
C4 C5 1.477(5) .
C6 C7 1.481(4) .
C7 C8 1.381(5) .
C8 C9 1.397(4) .
C8 H7 0.9500 .
C9 C8 1.397(4) 2_755
C9 H8 0.9500 .
