#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:41:43 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179151 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/12/4311283.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_4311283
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            'C73 H151 Cl9 Fe6 N6 O30'
_chemical_formula_weight         2247.15
_chemical_name_systematic
;
  ?
;
_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                   26.731(4)
_cell_length_b                   26.731(4)
_cell_length_c                   12.236(2)
_cell_measurement_reflns_used    14963
_cell_measurement_temperature    173(2)
_cell_volume                     7572(2)
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotatng anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0182
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16083
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         6.90
_exptl_absorpt_coefficient_mu    1.152
_exptl_absorpt_correction_T_max  0.8024
_exptl_absorpt_correction_T_min  0.6559
_exptl_absorpt_correction_type   'empirical (Scalepack)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3540
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         3374
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          1.534
_refine_ls_shift/su_mean         0.066
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0422P)²+24.7470P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.0940
_reflns_number_gt                3060
_reflns_number_total             3374
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049799wsi20040216_012135_17.cif
_cod_data_source_block           eu08
_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               4311283
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 0.120028(12) 0.117674(12) 0.00497(2) 0.01970(11) Uani 1 1 d . . .
Cl1 Cl 0.20325(2) 0.17605(2) 0.10580(5) 0.02848(15) Uani 1 1 d . . .
N1 N 0.15827(7) 0.17335(7) -0.14671(15) 0.0233(4) Uani 1 1 d . . .
O11 O 0.14810(6) 0.07246(6) -0.08142(12) 0.0235(3) Uani 1 1 d . . .
C11 C 0.17949(10) 0.09512(9) -0.18019(19) 0.0273(5) Uani 1 1 d . . .
H11A H 0.1536 0.0774 -0.2438 0.033 Uiso 1 1 calc R . .
H11B H 0.2112 0.0862 -0.1850 0.033 Uiso 1 1 calc R . .
C12 C 0.20398(9) 0.16011(9) -0.18048(19) 0.0276(5) Uani 1 1 d . . .
H12A H 0.2370 0.1787 -0.1293 0.033 Uiso 1 1 calc R . .
H12B H 0.2180 0.1756 -0.2546 0.033 Uiso 1 1 calc R . .
C13 C 0.05866(9) 0.09579(9) -0.20048(17) 0.0256(4) Uani 1 1 d . . .
H13A H 0.0242 0.0909 -0.2402 0.031 Uiso 1 1 calc R . .
H13B H 0.0655 0.0641 -0.2224 0.031 Uiso 1 1 calc R . .
O13 O 0.04871(6) 0.09329(6) -0.08662(12) 0.0215(3) Uani 1 1 d . . .
C14 C 0.11143(9) 0.15421(9) -0.23045(18) 0.0262(4) Uani 1 1 d . . .
H14A H 0.1265 0.1509 -0.3023 0.031 Uiso 1 1 calc R . .
H14B H 0.0995 0.1837 -0.2369 0.031 Uiso 1 1 calc R . .
C15 C 0.18240(9) 0.23576(9) -0.12021(19) 0.0271(5) Uani 1 1 d . . .
H15A H 0.2128 0.2466 -0.0641 0.033 Uiso 1 1 calc R . .
H15B H 0.1512 0.2405 -0.0871 0.033 Uiso 1 1 calc R . .
O16 O 0.25862(8) 0.27864(7) -0.25065(16) 0.0387(4) Uani 1 1 d . . .
C16 C 0.20803(10) 0.27801(10) -0.2147(2) 0.0325(5) Uani 1 1 d . . .
H16A H 0.1798 0.2660 -0.2752 0.039 Uiso 1 1 calc R . .
H16B H 0.2175 0.3171 -0.1907 0.039 Uiso 1 1 calc R . .
C17 C 0.28628(12) 0.31654(11) -0.3399(2) 0.0414(6) Uani 1 1 d . . .
H17A H 0.3052 0.3571 -0.3147 0.050 Uiso 1 1 calc R . .
H17B H 0.2574 0.3110 -0.3964 0.050 Uiso 1 1 calc R . .
C18 C 0.33013(13) 0.30383(12) -0.3866(3) 0.0495(7) Uani 1 1 d . . .
H18A H 0.3575 0.3362 -0.4334 0.059 Uiso 1 1 calc R . .
H18B H 0.3522 0.2985 -0.3272 0.059 Uiso 1 1 calc R . .
O18 O 0.30004(10) 0.25207(10) -0.4498(2) 0.0638(7) Uani 1 1 d . . .
C19 C 0.33805(17) 0.23570(17) -0.4931(4) 0.0789(12) Uani 1 1 d . . .
H19A H 0.3538 0.2228 -0.4330 0.095 Uiso 1 1 calc R . .
H19B H 0.3708 0.2695 -0.5286 0.095 Uiso 1 1 calc R . .
O20 O 0.2563(2) 0.13902(19) -0.5452(4) 0.0629(11) Uani 0.573(7) 1 d PD . .
O20' O 0.2844(3) 0.1299(3) -0.5163(5) 0.0629(11) Uani 0.43 1 d PD . .
C20 C 0.3089(2) 0.18809(17) -0.5746(4) 0.0850(14) Uani 1 1 d D . .
H20A H 0.3348 0.1746 -0.5949 0.102 Uiso 1 1 d R . .
H20B H 0.3020 0.2044 -0.6387 0.102 Uiso 1 1 d R . .
C21 C 0.2639(3) 0.1123(3) -0.4516(5) 0.0577(12) Uani 0.573(7) 1 d PD . .
H21A H 0.2681 0.1343 -0.3868 0.069 Uiso 0.573(7) 1 d PR . .
H21B H 0.2978 0.1090 -0.4608 0.069 Uiso 0.573(7) 1 d PR . .
C21' C 0.2268(4) 0.1116(3) -0.4845(7) 0.0577(12) Uani 0.43 1 d PD . .
H21C H 0.2040 0.1110 -0.5455 0.069 Uiso 0.427(7) 1 d PR . .
H21D H 0.2251 0.1355 -0.4276 0.069 Uiso 0.427(7) 1 d PR . .
C22 C 0.2072(2) 0.05081(17) -0.4467(3) 0.0787(12) Uani 1 1 d D . .
H22A H 0.2096 0.0297 -0.3854 0.118 Uiso 1 1 d R . .
H22B H 0.1739 0.0554 -0.4386 0.118 Uiso 1 1 d R . .
H22C H 0.2037 0.0300 -0.5128 0.118 Uiso 1 1 d R . .
Cl11 Cl 0.0663(3) 0.0143(5) -0.4949(5) 0.191(2) Uani 0.50 1 d P . .
C100 C 0.0000 0.0000 -0.4614(12) 0.095(5) Uani 0.50 3 d SP . .
H10A H 0.0000 0.0000 -0.3829 0.114 Uiso 0.50 3 d SPR . .
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11 Fe1 O13 99.92(6) 12 11 ?
O11 Fe1 O11 167.53(8) 12 . ?
O13 Fe1 O11 74.44(6) 11 . ?
O11 Fe1 O13 74.41(6) 12 . ?
O13 Fe1 O13 98.32(8) 11 . ?
O11 Fe1 O13 95.17(6) . . ?
O11 Fe1 N1 106.40(6) 12 . ?
O13 Fe1 N1 151.39(6) 11 . ?
O11 Fe1 N1 77.53(6) . . ?
O13 Fe1 N1 78.54(6) . . ?
O11 Fe1 Cl1 92.43(4) 12 . ?
O13 Fe1 Cl1 98.41(5) 11 . ?
O11 Fe1 Cl1 99.35(5) . . ?
O13 Fe1 Cl1 160.27(5) . . ?
N1 Fe1 Cl1 91.58(5) . . ?
C12 N1 C15 112.22(16) . . ?
C12 N1 C14 111.98(17) . . ?
C15 N1 C14 110.55(16) . . ?
C12 N1 Fe1 102.95(12) . . ?
C15 N1 Fe1 110.82(13) . . ?
C14 N1 Fe1 108.02(12) . . ?
C11 O11 Fe1 133.58(12) . 11 ?
C11 O11 Fe1 120.56(12) . . ?
Fe1 O11 Fe1 105.70(7) 11 . ?
O11 C11 C12 108.30(17) . . ?
N1 C12 C11 109.58(17) . . ?
O13 C13 C14 109.80(17) . . ?
C13 O13 Fe1 128.05(13) . 12 ?
C13 O13 Fe1 114.01(12) . . ?
Fe1 O13 Fe1 105.28(7) 12 . ?
N1 C14 C13 111.73(17) . . ?
N1 C15 C16 116.61(19) . . ?
C16 O16 C17 113.67(19) . . ?
O16 C16 C15 108.58(18) . . ?
O16 C17 C18 108.7(2) . . ?
O18 C18 C17 107.6(2) . . ?
C19 O18 C18 111.3(3) . . ?
O18 C19 C20 111.7(4) . . ?
O20' O20 C21' 88.5(7) . . ?
O20' O20 C20 77.7(5) . . ?
C21' O20 C20 150.5(7) . . ?
O20' O20 C21 41.5(5) . . ?
C21' O20 C21 48.1(5) . . ?
C20 O20 C21 110.3(5) . . ?
C21 O20' O20 95.8(7) . . ?
C21 O20' C21' 48.5(6) . . ?
O20 O20' C21' 48.6(5) . . ?
C21 O20' C20 138.2(7) . . ?
O20 O20' C20 64.2(5) . . ?
C21' O20' C20 108.6(6) . . ?
O20 C20 C19 118.4(4) . . ?
O20 C20 O20' 38.1(3) . . ?
C19 C20 O20' 109.4(4) . . ?
O20' C21 C21' 89.7(7) . . ?
O20' C21 O20 42.7(5) . . ?
C21' C21 O20 48.2(5) . . ?
O20' C21 C22 124.4(7) . . ?
C21' C21 C22 66.2(5) . . ?
O20 C21 C22 104.4(4) . . ?
O20 C21' C21 83.7(7) . . ?
O20 C21' O20' 42.9(4) . . ?
C21 C21' O20' 41.8(5) . . ?
O20 C21' C22 134.0(7) . . ?
C21 C21' C22 73.8(6) . . ?
O20' C21' C22 100.9(6) . . ?
C21' C22 C21 40.0(4) . . ?
Cl11 Cl11 Cl11 119.42(11) 12_554 11_554 ?
Cl11 Cl11 C100 62.33(14) 12_554 . ?
Cl11 Cl11 C100 62.33(14) 11_554 . ?
Cl11 Cl11 C100 60.17(12) 12_554 10_554 ?
Cl11 Cl11 C100 60.17(12) 11_554 10_554 ?
C100 Cl11 C100 32.5(10) . 10_554 ?
C100 C100 Cl11 75.8(5) 10_554 3 ?
C100 C100 Cl11 75.8(5) 10_554 . ?
Cl11 C100 Cl11 114.2(4) 3 . ?
C100 C100 Cl11 75.8(5) 10_554 2 ?
Cl11 C100 Cl11 114.2(4) 3 2 ?
Cl11 C100 Cl11 114.2(4) . 2 ?
C100 C100 Cl11 71.7(5) 10_554 10_554 ?
Cl11 C100 Cl11 57.50(16) 3 10_554 ?
Cl11 C100 Cl11 147.5(10) . 10_554 ?
Cl11 C100 Cl11 57.50(16) 2 10_554 ?
C100 C100 Cl11 71.7(5) 10_554 12_554 ?
Cl11 C100 Cl11 147.5(10) 3 12_554 ?
Cl11 C100 Cl11 57.50(16) . 12_554 ?
Cl11 C100 Cl11 57.50(16) 2 12_554 ?
Cl11 C100 Cl11 110.6(5) 10_554 12_554 ?
C100 C100 Cl11 71.7(5) 10_554 11_554 ?
Cl11 C100 Cl11 57.50(16) 3 11_554 ?
Cl11 C100 Cl11 57.50(16) . 11_554 ?
Cl11 C100 Cl11 147.5(10) 2 11_554 ?
Cl11 C100 Cl11 110.6(5) 10_554 11_554 ?
Cl11 C100 Cl11 110.6(5) 12_554 11_554 ?
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 O11 1.9773(14) 12 ?
Fe1 O13 1.9824(14) 11 ?
Fe1 O11 2.0120(14) . ?
Fe1 O13 2.0182(14) . ?
Fe1 N1 2.2767(18) . ?
Fe1 Cl1 2.3312(6) . ?
N1 C12 1.491(3) . ?
N1 C15 1.493(3) . ?
N1 C14 1.496(3) . ?
O11 C11 1.422(2) . ?
O11 Fe1 1.9773(14) 11 ?
C11 C12 1.520(3) . ?
C13 O13 1.414(3) . ?
C13 C14 1.536(3) . ?
O13 Fe1 1.9824(14) 12 ?
C15 C16 1.519(3) . ?
O16 C16 1.414(3) . ?
O16 C17 1.420(3) . ?
C17 C18 1.488(4) . ?
C18 O18 1.431(4) . ?
O18 C19 1.396(4) . ?
C19 C20 1.493(6) . ?
O20 O20' 0.966(7) . ?
O20 C21' 1.064(9) . ?
O20 C20 1.409(6) . ?
O20 C21 1.418(7) . ?
O20' C21 0.945(8) . ?
O20' C21' 1.417(10) . ?
O20' C20 1.528(7) . ?
C21 C21' 1.062(10) . ?
C21 C22 1.585(8) . ?
C21' C22 1.510(9) . ?
Cl11 Cl11 1.621(5) 12_554 ?
Cl11 Cl11 1.621(5) 11_554 ?
Cl11 C100 1.668(6) . ?
Cl11 C100 1.702(7) 10_554 ?
C100 C100 0.94(3) 10_554 ?
C100 Cl11 1.668(6) 3 ?
C100 Cl11 1.668(6) 2 ?
C100 Cl11 1.702(7) 10_554 ?
C100 Cl11 1.702(7) 12_554 ?
C100 Cl11 1.702(7) 11_554 ?
