#------------------------------------------------------------------------------
#$Date: 2025-08-20 23:21:57 +0200 (Wed 20 de Aug de 2025) $
#$Revision: 301837 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/12/4311274.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_4311274
loop_
_publ_author_name
'Rolf W. Saalfrank'
'Christian Deutscher'
'Stefan Sperner'
'Takayuki Nakajima'
'Ayuk M. Ako'
'Eveline Uller'
'Frank Hampel'
'Frank W. Heinemann'
_publ_contact_author             'Dr. Frank Hampel'
_publ_contact_author_email       hampel@organik.uni-erlangen.de
_publ_section_title
;
 Six-Membered Metalla-coronands. Synthesis and Crystal Packing: Columns,
 Compartments, and 3D-Networks,
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4372
_journal_page_last               4382
_journal_paper_doi               10.1021/ic049799w
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C102 H150 Fe6 N12 O30 S6'
_chemical_formula_weight         2551.80
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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            3
_cell_length_a                   25.0845(6)
_cell_length_b                   25.0845(6)
_cell_length_c                   16.0454(7)
_cell_measurement_reflns_used    4354
_cell_measurement_temperature    173(2)
_cell_volume                     8743.6(5)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'SHELXTL NT'
_computing_publication_material  'SHELXTL NT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0459
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9523
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    0.913
_exptl_absorpt_correction_T_max  0.8385
_exptl_absorpt_correction_T_min  0.7406
_exptl_absorpt_correction_type   'empirical (Scalepack)'
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       orange
_exptl_crystal_F_000             4014
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4168
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0664P)²+9.4776P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1138
_reflns_number_gt                3316
_reflns_number_total             4168
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049799wsi20040216_012135_08.cif
_cod_data_source_block           tn04
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Rhombohedral' changed to 'rhombohedral'
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_original_sg_symbol_H-M      'R -3'
_cod_database_code               4311274
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 0.910650(12) 0.054054(12) 0.505034(18) 0.02739(12) Uani 1 1 d . . .
O1 O 0.85297(6) -0.02122(6) 0.43938(9) 0.0310(3) Uani 1 1 d . . .
C2 C 0.82365(10) -0.01574(10) 0.36619(15) 0.0371(5) Uani 1 1 d . . .
H2A H 0.7805 -0.0499 0.3637 0.045 Uiso 1 1 calc R . .
H2B H 0.8454 -0.0177 0.3158 0.045 Uiso 1 1 calc R . .
C3 C 0.82548(10) 0.04552(10) 0.36993(16) 0.0388(5) Uani 1 1 d . . .
H3A H 0.8148 0.0552 0.3147 0.047 Uiso 1 1 calc R . .
H3B H 0.7950 0.0433 0.4110 0.047 Uiso 1 1 calc R . .
N4 N 0.88845(8) 0.09477(8) 0.39460(12) 0.0338(4) Uani 1 1 d . . .
C5 C 0.93496(10) 0.10708(11) 0.32842(14) 0.0374(5) Uani 1 1 d . . .
H5A H 0.9638 0.1520 0.3247 0.045 Uiso 1 1 calc R . .
H5B H 0.9138 0.0930 0.2740 0.045 Uiso 1 1 calc R . .
C6 C 0.97170(10) 0.07403(10) 0.34617(13) 0.0350(5) Uani 1 1 d . . .
H6A H 0.9476 0.0306 0.3281 0.042 Uiso 1 1 calc R . .
H6B H 1.0108 0.0941 0.3144 0.042 Uiso 1 1 calc R . .
O7 O 0.98440(6) 0.07667(6) 0.43280(9) 0.0287(3) Uani 1 1 d . . .
C8 C 0.89026(11) 0.15292(10) 0.42113(17) 0.0419(5) Uani 1 1 d . . .
H8A H 0.9323 0.1820 0.4412 0.050 Uiso 1 1 calc R . .
H8B H 0.8620 0.1432 0.4690 0.050 Uiso 1 1 calc R . .
C9 C 0.87326(12) 0.18540(12) 0.35522(19) 0.0513(6) Uani 1 1 d . . .
H9A H 0.8848 0.2273 0.3744 0.062 Uiso 1 1 calc R . .
H9B H 0.8957 0.1891 0.3029 0.062 Uiso 1 1 calc R . .
O10 O 0.80974(8) 0.15115(8) 0.34116(11) 0.0457(4) Uani 1 1 d . . .
C11 C 0.78929(16) 0.17304(15) 0.27372(18) 0.0569(7) Uani 1 1 d . . .
H11A H 0.8221 0.1924 0.2312 0.068 Uiso 1 1 calc R . .
H11B H 0.7792 0.2043 0.2938 0.068 Uiso 1 1 calc R . .
C12 C 0.73352(16) 0.11967(18) 0.23682(19) 0.0651(9) Uani 1 1 d . . .
H12A H 0.7009 0.0998 0.2795 0.078 Uiso 1 1 calc R . .
H12B H 0.7174 0.1336 0.1904 0.078 Uiso 1 1 calc R . .
O13 O 0.75127(9) 0.07733(11) 0.20696(14) 0.0605(5) Uani 1 1 d . . .
C14 C 0.70412(14) 0.02546(18) 0.1642(2) 0.0705(9) Uani 1 1 d . . .
H14A H 0.7002 0.0371 0.1066 0.085 Uiso 1 1 calc R . .
H14B H 0.6642 0.0107 0.1930 0.085 Uiso 1 1 calc R . .
C15 C 0.72006(15) -0.02391(17) 0.1627(2) 0.0685(9) Uani 1 1 d . . .
H15A H 0.7254 -0.0347 0.2203 0.082 Uiso 1 1 calc R . .
H15B H 0.6867 -0.0612 0.1358 0.082 Uiso 1 1 calc R . .
O16 O 0.77613(11) -0.00197(11) 0.11684(14) 0.0666(6) Uani 1 1 d . . .
C21 C 0.80529(15) -0.03493(14) 0.12354(18) 0.0576(7) Uani 1 1 d . . .
C22 C 0.78061(16) -0.09250(15) 0.16237(19) 0.0640(8) Uani 1 1 d . . .
H22A H 0.7406 -0.1114 0.1863 0.077 Uiso 1 1 calc R . .
C23 C 0.81512(18) -0.12140(17) 0.1655(2) 0.0694(9) Uani 1 1 d . . .
H23A H 0.7986 -0.1605 0.1915 0.083 Uiso 1 1 calc R . .
C24 C 0.8729(2) -0.09438(19) 0.1315(2) 0.0804(10) Uani 1 1 d . . .
H24A H 0.8970 -0.1138 0.1351 0.097 Uiso 1 1 calc R . .
C25 C 0.8949(2) -0.0393(2) 0.0925(3) 0.0966(14) Uani 1 1 d . . .
H25A H 0.9343 -0.0212 0.0667 0.116 Uiso 1 1 calc R . .
C26 C 0.86233(18) -0.00902(17) 0.0891(3) 0.0785(10) Uani 1 1 d . . .
H26A H 0.8795 0.0300 0.0627 0.094 Uiso 1 1 calc R . .
S100 S 0.76822(4) 0.07247(5) 0.68543(6) 0.0756(3) Uani 1 1 d . . .
N100 N 0.84801(9) 0.06280(9) 0.57488(13) 0.0389(4) Uani 1 1 d . . .
C100 C 0.81506(11) 0.06764(11) 0.62122(15) 0.0390(5) Uani 1 1 d . . .
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'
S S 0.1246 0.1234 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 O7 102.15(6) 11_666 12_546 ?
O1 Fe1 O1 169.84(7) 11_666 . ?
O7 Fe1 O1 75.13(6) 12_546 . ?
O1 Fe1 O7 75.38(6) 11_666 . ?
O7 Fe1 O7 99.33(8) 12_546 . ?
O1 Fe1 O7 95.25(6) . . ?
O1 Fe1 N100 90.92(7) 11_666 . ?
O7 Fe1 N100 97.36(7) 12_546 . ?
O1 Fe1 N100 99.12(7) . . ?
O7 Fe1 N100 160.28(7) . . ?
O1 Fe1 N4 103.91(6) 11_666 . ?
O7 Fe1 N4 152.68(6) 12_546 . ?
O1 Fe1 N4 77.78(6) . . ?
O7 Fe1 N4 79.60(6) . . ?
N100 Fe1 N4 90.29(8) . . ?
C2 O1 Fe1 134.84(13) . 12_546 ?
C2 O1 Fe1 120.28(12) . . ?
Fe1 O1 Fe1 104.72(6) 12_546 . ?
O1 C2 C3 108.01(18) . . ?
N4 C3 C2 109.43(16) . . ?
C3 N4 C5 112.17(18) . . ?
C3 N4 C8 112.68(17) . . ?
C5 N4 C8 111.16(18) . . ?
C3 N4 Fe1 103.47(12) . . ?
C5 N4 Fe1 108.01(12) . . ?
C8 N4 Fe1 108.92(14) . . ?
N4 C5 C6 111.89(17) . . ?
O7 C6 C5 109.63(17) . . ?
C6 O7 Fe1 127.92(12) . 11_666 ?
C6 O7 Fe1 113.45(12) . . ?
Fe1 O7 Fe1 104.28(6) 11_666 . ?
N4 C8 C9 116.4(2) . . ?
O10 C9 C8 108.7(2) . . ?
C9 O10 C11 113.9(2) . . ?
O10 C11 C12 108.2(2) . . ?
O13 C12 C11 107.5(2) . . ?
C14 O13 C12 114.7(2) . . ?
O13 C14 C15 108.9(2) . . ?
O16 C15 C14 108.2(3) . . ?
C21 O16 C15 116.8(3) . . ?
O16 C21 C26 115.9(3) . . ?
O16 C21 C22 124.7(3) . . ?
C26 C21 C22 119.4(3) . . ?
C23 C22 C21 119.2(3) . . ?
C22 C23 C24 120.8(4) . . ?
C25 C24 C23 118.6(4) . . ?
C24 C25 C26 122.1(4) . . ?
C21 C26 C25 119.8(4) . . ?
C100 N100 Fe1 173.7(2) . . ?
N100 C100 S100 178.5(2) . . ?
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 O1 1.9697(14) 11_666 ?
Fe1 O7 1.9813(14) 12_546 ?
Fe1 O1 2.0091(14) . ?
Fe1 O7 2.0095(14) . ?
Fe1 N100 2.0293(19) . ?
Fe1 N4 2.2499(18) . ?
O1 C2 1.428(3) . ?
O1 Fe1 1.9697(14) 12_546 ?
C2 C3 1.516(3) . ?
C3 N4 1.492(3) . ?
N4 C5 1.491(3) . ?
N4 C8 1.498(3) . ?
C5 C6 1.543(3) . ?
C6 O7 1.420(3) . ?
O7 Fe1 1.9813(14) 11_666 ?
C8 C9 1.520(3) . ?
C9 O10 1.400(3) . ?
O10 C11 1.421(3) . ?
C11 C12 1.492(5) . ?
C12 O13 1.424(4) . ?
O13 C14 1.422(4) . ?
C14 C15 1.480(6) . ?
C15 O16 1.431(4) . ?
O16 C21 1.354(4) . ?
C21 C26 1.358(5) . ?
C21 C22 1.401(5) . ?
C22 C23 1.380(5) . ?
C23 C24 1.369(6) . ?
C24 C25 1.358(6) . ?
C25 C26 1.367(6) . ?
S100 C100 1.612(2) . ?
N100 C100 1.162(3) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Fe1 O1 C2 -105.7(3) 11_666 . . . ?
O7 Fe1 O1 C2 178.52(16) 12_546 . . . ?
O7 Fe1 O1 C2 -83.20(15) . . . . ?
N100 Fe1 O1 C2 83.26(16) . . . . ?
N4 Fe1 O1 C2 -5.05(15) . . . . ?
O1 Fe1 O1 Fe1 70.3(2) 11_666 . . 12_546 ?
O7 Fe1 O1 Fe1 -5.46(6) 12_546 . . 12_546 ?
O7 Fe1 O1 Fe1 92.82(7) . . . 12_546 ?
N100 Fe1 O1 Fe1 -100.72(8) . . . 12_546 ?
N4 Fe1 O1 Fe1 170.97(8) . . . 12_546 ?
Fe1 O1 C2 C3 165.48(15) 12_546 . . . ?
Fe1 O1 C2 C3 -19.9(2) . . . . ?
O1 C2 C3 N4 45.9(3) . . . . ?
C2 C3 N4 C5 68.5(2) . . . . ?
C2 C3 N4 C8 -165.1(2) . . . . ?
C2 C3 N4 Fe1 -47.6(2) . . . . ?
O1 Fe1 N4 C3 -161.71(13) 11_666 . . . ?
O7 Fe1 N4 C3 36.1(2) 12_546 . . . ?
O1 Fe1 N4 C3 28.58(13) . . . . ?
O7 Fe1 N4 C3 126.34(14) . . . . ?
N100 Fe1 N4 C3 -70.69(14) . . . . ?
O1 Fe1 N4 C5 79.22(14) 11_666 . . . ?
O7 Fe1 N4 C5 -82.96(19) 12_546 . . . ?
O1 Fe1 N4 C5 -90.49(14) . . . . ?
O7 Fe1 N4 C5 7.27(13) . . . . ?
N100 Fe1 N4 C5 170.24(14) . . . . ?
O1 Fe1 N4 C8 -41.62(15) 11_666 . . . ?
O7 Fe1 N4 C8 156.20(14) 12_546 . . . ?
O1 Fe1 N4 C8 148.67(15) . . . . ?
O7 Fe1 N4 C8 -113.57(14) . . . . ?
N100 Fe1 N4 C8 49.40(15) . . . . ?
C3 N4 C5 C6 -98.9(2) . . . . ?
C8 N4 C5 C6 133.93(19) . . . . ?
Fe1 N4 C5 C6 14.5(2) . . . . ?
N4 C5 C6 O7 -39.1(2) . . . . ?
C5 C6 O7 Fe1 -85.66(19) . . . 11_666 ?
C5 C6 O7 Fe1 47.09(19) . . . . ?
O1 Fe1 O7 C6 -137.85(14) 11_666 . . . ?
O7 Fe1 O7 C6 121.92(13) 12_546 . . . ?
O1 Fe1 O7 C6 46.16(13) . . . . ?
N100 Fe1 O7 C6 -90.6(2) . . . . ?
N4 Fe1 O7 C6 -30.36(13) . . . . ?
O1 Fe1 O7 Fe1 5.44(6) 11_666 . . 11_666 ?
O7 Fe1 O7 Fe1 -94.79(6) 12_546 . . 11_666 ?
O1 Fe1 O7 Fe1 -170.55(6) . . . 11_666 ?
N100 Fe1 O7 Fe1 52.7(2) . . . 11_666 ?
N4 Fe1 O7 Fe1 112.93(7) . . . 11_666 ?
C3 N4 C8 C9 -62.9(3) . . . . ?
C5 N4 C8 C9 64.0(3) . . . . ?
Fe1 N4 C8 C9 -177.12(17) . . . . ?
N4 C8 C9 O10 72.4(3) . . . . ?
C8 C9 O10 C11 -173.0(2) . . . . ?
C9 O10 C11 C12 150.6(2) . . . . ?
O10 C11 C12 O13 -61.4(3) . . . . ?
C11 C12 O13 C14 -175.7(2) . . . . ?
C12 O13 C14 C15 -160.5(3) . . . . ?
O13 C14 C15 O16 -62.7(3) . . . . ?
C14 C15 O16 C21 166.1(3) . . . . ?
C15 O16 C21 C26 -171.3(3) . . . . ?
C15 O16 C21 C22 9.0(4) . . . . ?
O16 C21 C22 C23 -179.7(3) . . . . ?
C26 C21 C22 C23 0.6(5) . . . . ?
C21 C22 C23 C24 0.2(5) . . . . ?
C22 C23 C24 C25 -1.8(6) . . . . ?
C23 C24 C25 C26 2.6(7) . . . . ?
O16 C21 C26 C25 -179.6(4) . . . . ?
C22 C21 C26 C25 0.1(6) . . . . ?
C24 C25 C26 C21 -1.8(7) . . . . ?
O1 Fe1 N100 C100 -54.2(17) 11_666 . . . ?
O7 Fe1 N100 C100 48.2(17) 12_546 . . . ?
O1 Fe1 N100 C100 124.2(17) . . . . ?
O7 Fe1 N100 C100 -99.5(17) . . . . ?
N4 Fe1 N100 C100 -158.1(17) . . . . ?
Fe1 N100 C100 S100 -94(9) . . . . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168337096
