#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:13:21 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179472 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/69/4336944.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_4336944
loop_
_publ_author_name
'M. Menelaou'
'E. Vournari'
'V. Psycharis'
'C. P. Raptopoulou'
'A. Terzis'
'V. Tangoulis'
'Y. Sanakis'
'C. Mateescu'
'A. Salifoglou'
_publ_section_title
;
 Heptanuclear Antiferromagnetic Fe(III)-d-(-)-Quinato Assemblies with an
 S= 3/2 Ground State-pH-Specific Synthetic Chemistry, Spectroscopic,
 Structural, and Magnetic Susceptibility Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13849
_journal_page_last               13860
_journal_paper_doi               10.1021/ic401036e
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C42 H106 Fe7 N O68 S2'
_chemical_formula_weight         2168.35
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           182
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c 2c'
_symmetry_space_group_name_H-M   'P 63 2 2'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   16.2964(3)
_cell_length_b                   16.2964(3)
_cell_length_c                   18.6865(3)
_cell_measurement_reflns_used    31564
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      72.06
_cell_measurement_theta_min      6.70
_cell_volume                     4297.76(13)
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            35313
_diffrn_reflns_theta_full        65.00
_diffrn_reflns_theta_max         65.00
_diffrn_reflns_theta_min         6.71
_exptl_absorpt_coefficient_mu    10.733
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.268
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2246
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.021(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         2392
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0446
_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)+(0.0838P)²+3.6495P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1273
_refine_ls_wR_factor_ref         0.1320
_reflns_number_gt                2168
_reflns_number_total             2392
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401036e_si_005.cif
_cod_data_source_block           salfeq309
_cod_database_code               4336944
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, -x, -z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -x+y, -z'
'-y, x-y, z'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x+y, -x, z'
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 0.3333 0.6667 0.2500 0.0191(3) Uani 1 6 d S
Fe2 Fe 0.22180(3) 0.77820(3) 0.2500 0.0264(3) Uani 1 2 d S
Fe3 Fe 0.10425(5) 0.55213(3) 0.2500 0.0227(2) Uani 1 2 d S
O1 O 0.1956(2) 0.3571(2) 0.33203(19) 0.0449(9) Uani 1 1 d .
O2 O 0.10666(19) 0.43893(19) 0.28830(14) 0.0300(6) Uani 1 1 d .
O3 O 0.1109(3) 0.2994(3) 0.4316(3) 0.0779(15) Uani 1 1 d .
O4 O 0.0195(2) 0.5393(3) 0.33091(18) 0.0410(8) Uani 1 1 d .
H4O H -0.0236 0.5530 0.3206 0.057 Uiso 1 1 d .
O5 O -0.1706(3) 0.4290(4) 0.3650(2) 0.0849(17) Uani 1 1 d .
H5O H -0.2231 0.3937 0.3847 0.119 Uiso 1 1 calc R
O6 O -0.1981(3) 0.2520(4) 0.3152(4) 0.112(2) Uani 1 1 d .
H6O H -0.2396 0.2681 0.3164 0.156 Uiso 1 1 d .
O7 O 0.22281(19) 0.6671(2) 0.3029(2) 0.0236(7) Uani 1 1 d .
H7O H 0.227(3) 0.671(4) 0.337(3) 0.023(17) Uiso 1 1 d .
C1 C 0.1277(3) 0.3429(4) 0.3742(3) 0.0507(14) Uani 1 1 d .
C2 C 0.0658(3) 0.3854(3) 0.3518(3) 0.0405(12) Uani 1 1 d .
C3 C 0.0635(4) 0.4475(5) 0.4094(3) 0.0517(15) Uani 1 1 d .
C4 C -0.0085(3) 0.4793(5) 0.3928(3) 0.0534(16) Uani 1 1 d .
H4 H -0.006(5) 0.535(5) 0.431(4) 0.080 Uiso 1 1 d .
C5 C -0.1066(4) 0.3964(6) 0.3820(4) 0.070(2) Uani 1 1 d .
C6 C -0.1068(4) 0.3335(5) 0.3229(4) 0.069(2) Uani 1 1 d .
C7 C -0.0330(3) 0.3017(4) 0.3364(3) 0.0603(16) Uani 1 1 d .
H7A H -0.0539 0.2575 0.3775 0.078 Uiso 1 1 calc R
H7B H -0.0299 0.2672 0.2938 0.078 Uiso 1 1 calc R
S S 0.3333 0.6667 0.47195(9) 0.0282(4) Uani 1 3 d S
O11 O 0.3333 0.6667 0.5511(2) 0.0297(10) Uani 1 3 d S
O12 O 0.2554(2) 0.6798(2) 0.44608(18) 0.0387(8) Uani 1 1 d .
H3A H 0.129(4) 0.505(4) 0.417(3) 0.057(16) Uiso 1 1 d .
H3B H 0.037(4) 0.406(4) 0.460(3) 0.046(14) Uiso 1 1 d .
H5 H -0.115(4) 0.354(4) 0.438(3) 0.066(17) Uiso 1 1 d .
H6 H -0.096(4) 0.363(4) 0.280(3) 0.052(17) Uiso 1 1 d .
N N 0.6667 0.3333 0.2500 0.056(3) Uani 1 6 d S
O1W O 0.6620(5) 0.9615(4) 0.6388(3) 0.0970(18) Uani 1 1 d .
O2W O 0.5900(6) 0.8285(6) 0.5328(4) 0.054(2) Uani 0.50 1 d P
O3W O 0.5990(7) 0.8878(6) 0.5008(5) 0.075(3) Uani 0.50 1 d P
O4W O 0.1311(14) 1.0000 0.5000 0.108(6) Uiso 0.40 2 d SP
O5W O 0.8433(17) 0.9883(16) 0.6461(11) 0.154(7) Uiso 0.40 1 d P
O6W O -0.0047(14) 0.1436(14) 0.2183 0.139(6) Uiso 0.40 1 d P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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 80.87(18) 3_665 .
O7 Fe1 O7 81.38(18) 3_665 12_565
O7 Fe1 O7 98.87(13) . 12_565
O7 Fe1 O7 98.87(13) 3_665 7_565
O7 Fe1 O7 81.38(18) . 7_565
O7 Fe1 O7 179.67(16) 12_565 7_565
O7 Fe1 O7 98.87(13) 3_665 6
O7 Fe1 O7 179.67(16) . 6
O7 Fe1 O7 80.87(18) 12_565 6
O7 Fe1 O7 98.87(13) 7_565 6
O7 Fe1 O7 179.67(16) 3_665 9_665
O7 Fe1 O7 98.87(13) . 9_665
O7 Fe1 O7 98.87(13) 12_565 9_665
O7 Fe1 O7 80.87(18) 7_565 9_665
O7 Fe1 O7 81.38(18) 6 9_665
O2 Fe2 O2 176.17(16) 12_565 7_565
O2 Fe2 O1 80.16(12) 12_565 12_565
O2 Fe2 O1 97.45(12) 7_565 12_565
O2 Fe2 O1 97.45(12) 12_565 7_565
O2 Fe2 O1 80.16(12) 7_565 7_565
O1 Fe2 O1 103.8(2) 12_565 7_565
O2 Fe2 O7 104.84(12) 12_565 .
O2 Fe2 O7 78.16(11) 7_565 .
O1 Fe2 O7 92.37(14) 12_565 .
O1 Fe2 O7 154.41(14) 7_565 .
O2 Fe2 O7 78.16(12) 12_565 3_665
O2 Fe2 O7 104.84(12) 7_565 3_665
O1 Fe2 O7 154.41(14) 12_565 3_665
O1 Fe2 O7 92.37(14) 7_565 3_665
O7 Fe2 O7 80.27(17) . 3_665
O4 Fe3 O4 105.97(19) 7_565 .
O4 Fe3 O2 87.94(12) 7_565 7_565
O4 Fe3 O2 93.24(12) . 7_565
O4 Fe3 O2 93.24(12) 7_565 .
O4 Fe3 O2 87.94(12) . .
O2 Fe3 O2 178.05(16) 7_565 .
O4 Fe3 O7 157.33(13) 7_565 .
O4 Fe3 O7 90.96(14) . .
O2 Fe3 O7 75.92(11) 7_565 .
O2 Fe3 O7 102.51(12) . .
O4 Fe3 O7 90.96(14) 7_565 7_565
O4 Fe3 O7 157.33(13) . 7_565
O2 Fe3 O7 102.51(12) 7_565 7_565
O2 Fe3 O7 75.92(11) . 7_565
O7 Fe3 O7 77.43(17) . 7_565
C1 O1 Fe2 117.7(3) . 7_565
C2 O2 Fe2 118.0(3) . 7_565
C2 O2 Fe3 130.1(3) . .
Fe2 O2 Fe3 106.97(12) 7_565 .
C4 O4 Fe3 130.8(3) . .
C4 O4 H4O 109.6 . .
Fe3 O4 H4O 114.7 . .
C5 O5 H5O 109.5 . .
C6 O6 H6O 109.7 . .
Fe1 O7 Fe2 99.43(15) . .
Fe1 O7 Fe3 100.60(14) . .
Fe2 O7 Fe3 98.44(14) . .
Fe1 O7 H7O 116(4) . .
Fe2 O7 H7O 115(5) . .
Fe3 O7 H7O 123(5) . .
O3 C1 O1 124.1(5) . .
O3 C1 C2 119.0(5) . .
O1 C1 C2 116.9(4) . .
O2 C2 C3 110.4(4) . .
O2 C2 C7 110.5(4) . .
C3 C2 C7 111.7(5) . .
O2 C2 C1 106.9(4) . .
C3 C2 C1 110.7(4) . .
C7 C2 C1 106.5(4) . .
C2 C3 C4 111.5(4) . .
C2 C3 H3A 111(3) . .
C4 C3 H3A 110(3) . .
C2 C3 H3B 109(3) . .
C4 C3 H3B 104(3) . .
H3A C3 H3B 111(4) . .
O4 C4 C5 109.7(4) . .
O4 C4 C3 110.9(4) . .
C5 C4 C3 111.9(5) . .
O4 C4 H4 95(3) . .
C5 C4 H4 114(4) . .
C3 C4 H4 114(4) . .
O5 C5 C4 110.1(6) . .
O5 C5 C6 109.7(6) . .
C4 C5 C6 110.4(5) . .
O5 C5 H5 121(3) . .
C4 C5 H5 99(3) . .
C6 C5 H5 106(3) . .
O6 C6 C5 110.8(6) . .
O6 C6 C7 109.2(6) . .
C5 C6 C7 111.7(5) . .
O6 C6 H6 104(4) . .
C5 C6 H6 111(4) . .
C7 C6 H6 110(4) . .
C2 C7 C6 112.3(5) . .
C2 C7 H7A 109.1 . .
C6 C7 H7A 109.1 . .
C2 C7 H7B 109.1 . .
C6 C7 H7B 109.1 . .
H7A C7 H7B 107.9 . .
O12 S O12 109.77(14) . 12_565
O12 S O12 109.77(14) . 9_665
O12 S O12 109.77(14) 12_565 9_665
O12 S O11 109.17(14) . .
O12 S O11 109.17(14) 12_565 .
O12 S O11 109.17(14) 9_665 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O7 2.057(3) 3_665
Fe1 O7 2.057(3) .
Fe1 O7 2.057(3) 12_565
Fe1 O7 2.057(3) 7_565
Fe1 O7 2.057(3) 6
Fe1 O7 2.057(3) 9_665
Fe2 O2 1.974(3) 12_565
Fe2 O2 1.974(3) 7_565
Fe2 O1 1.979(3) 12_565
Fe2 O1 1.979(3) 7_565
Fe2 O7 2.070(3) .
Fe2 O7 2.070(3) 3_665
Fe3 O4 1.987(3) 7_565
Fe3 O4 1.987(3) .
Fe3 O2 1.997(3) 7_565
Fe3 O2 1.997(3) .
Fe3 O7 2.144(3) .
Fe3 O7 2.144(3) 7_565
O1 C1 1.280(7) .
O1 Fe2 1.979(3) 7_565
O2 C2 1.426(5) .
O2 Fe2 1.974(3) 7_565
O3 C1 1.239(6) .
O4 C4 1.434(6) .
O4 H4O 0.8575 .
O5 C5 1.423(7) .
O5 H5O 0.8400 .
O6 C6 1.422(7) .
O6 H6O 0.8386 .
O7 H7O 0.64(5) .
C1 C2 1.540(7) .
C2 C3 1.492(8) .
C2 C7 1.530(6) .
C3 C4 1.534(7) .
C3 H3A 1.02(6) .
C3 H3B 1.12(5) .
C4 C5 1.503(9) .
C4 H4 1.14(7) .
C5 C6 1.507(11) .
C5 H5 1.22(6) .
C6 C7 1.550(9) .
C6 H6 0.90(6) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
S O12 1.472(3) .
S O12 1.472(3) 12_565
S O12 1.472(3) 9_665
S O11 1.479(5) .
O2W O3W 1.081(10) .
O5W O6W 1.36(2) 11_665
O6W O5W 1.36(2) 10_454
