#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:41:43 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179151 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/12/4311275.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_4311275
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            'C85 H115 Cl15 Fe6 N12 O18 S6'
_chemical_formula_weight         2652.10
_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                   29.0350(7)
_cell_length_b                   29.0350(7)
_cell_length_c                   11.8571(5)
_cell_measurement_reflns_used    6107
_cell_measurement_temperature    173(2)
_cell_volume                     8656.7(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 0.890
_diffrn_measured_fraction_theta_max 0.890
_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  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8460
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    1.254
_exptl_absorpt_correction_T_max  0.7876
_exptl_absorpt_correction_T_min  0.6681
_exptl_absorpt_correction_type   'empirical (Scalepack)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4080
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.641
_refine_diff_density_min         -1.130
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.846
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3932
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.861
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0817
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2400
_refine_ls_wR_factor_ref         0.2556
_reflns_number_gt                3121
_reflns_number_total             3932
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049799wsi20040216_012135_09.cif
_cod_data_source_block           tn05
_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               4311275
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 -0.37249(2) 0.21002(2) -0.16954(5) 0.0263(3) Uani 1 1 d . . .
O1 O -0.30531(12) 0.23250(12) -0.0815(3) 0.0298(7) Uani 1 1 d . . .
C2 C -0.30648(18) 0.20692(18) 0.0221(4) 0.0325(9) Uani 1 1 d . . .
H2A H -0.3064 0.2285 0.0867 0.039 Uiso 1 1 calc R . .
H2B H -0.2748 0.2026 0.0280 0.039 Uiso 1 1 calc R . .
C3 C -0.35717(19) 0.15253(18) 0.0229(4) 0.0336(10) Uani 1 1 d . . .
H3A H -0.3531 0.1282 -0.0294 0.040 Uiso 1 1 calc R . .
H3B H -0.3634 0.1371 0.0996 0.040 Uiso 1 1 calc R . .
N4 N -0.40360(15) 0.15820(14) -0.0124(3) 0.0300(8) Uani 1 1 d . . .
C5 C -0.4177(2) 0.18762(18) 0.0715(4) 0.0329(9) Uani 1 1 d . . .
H5A H -0.4050 0.1845 0.1471 0.040 Uiso 1 1 calc R . .
H5B H -0.4569 0.1712 0.0751 0.040 Uiso 1 1 calc R . .
C6 C -0.39313(18) 0.24628(17) 0.0407(4) 0.0294(9) Uani 1 1 d . . .
H6A H -0.4119 0.2619 0.0811 0.035 Uiso 1 1 calc R . .
H6B H -0.3553 0.2658 0.0638 0.035 Uiso 1 1 calc R . .
O7 O -0.39707(12) 0.25143(12) -0.0773(3) 0.0280(6) Uani 1 1 d . . .
C8 C -0.45086(19) 0.10535(17) -0.0382(4) 0.0373(10) Uani 1 1 d . . .
H8A H -0.4408 0.0878 -0.0971 0.045 Uiso 1 1 calc R . .
H8B H -0.4791 0.1111 -0.0699 0.045 Uiso 1 1 calc R . .
C9 C -0.4737(2) 0.0677(2) 0.0627(5) 0.0426(12) Uani 1 1 d . . .
H9A H -0.4725 0.0878 0.1312 0.051 Uiso 1 1 calc R . .
H9B H -0.5111 0.0403 0.0481 0.051 Uiso 1 1 calc R . .
O10 O -0.44147(16) 0.04311(14) 0.0779(3) 0.0453(9) Uani 1 1 d . . .
C11 C -0.4467(3) 0.01681(18) 0.1764(5) 0.0498(14) Uani 1 1 d . . .
C12 C -0.4858(3) 0.0047(2) 0.2556(5) 0.0577(16) Uani 1 1 d . . .
H12A H -0.5124 0.0142 0.2448 0.069 Uiso 1 1 calc R . .
C13 C -0.4846(4) -0.0227(3) 0.3553(6) 0.081(3) Uani 1 1 d . . .
H13A H -0.5114 -0.0323 0.4109 0.097 Uiso 1 1 calc R . .
C14 C -0.4458(4) -0.0354(3) 0.3716(8) 0.082(3) Uani 1 1 d . . .
H14A H -0.4451 -0.0524 0.4397 0.099 Uiso 1 1 calc R . .
C15 C -0.4091(5) -0.0244(3) 0.2941(9) 0.092(3) Uani 1 1 d . . .
H15A H -0.3827 -0.0341 0.3069 0.110 Uiso 1 1 calc R . .
C16 C -0.4082(3) 0.0013(3) 0.1931(7) 0.0678(19) Uani 1 1 d . . .
H16A H -0.3823 0.0080 0.1370 0.081 Uiso 1 1 calc R . .
N10 N -0.37479(13) 0.14570(13) -0.2633(3) 0.0240(7) Uani 1 1 d . . .
S10 S -0.36554(11) 0.06253(10) -0.3269(2) 0.0894(8) Uani 1 1 d . . .
C10 C -0.3713(2) 0.1144(3) -0.2819(5) 0.0573(17) Uani 1 1 d . . .
C100 C -0.1907(3) 0.0289(3) 0.0593(8) 0.096(3) Uani 1 1 d D . .
H10A H -0.2044 0.0478 0.0177 0.115 Uiso 1 1 d R . .
H10B H -0.2060 0.0220 0.1335 0.115 Uiso 1 1 d R . .
Cl11 Cl -0.1240(2) 0.0662(2) 0.0703(4) 0.1082(12) Uani 0.634(7) 1 d PD . .
Cl1A Cl -0.1285(3) 0.0331(4) 0.0408(7) 0.1082(12) Uani 0.37 1 d PD . .
Cl12 Cl -0.2099(2) -0.0331(2) -0.0086(4) 0.1082(12) Uani 0.634(7) 1 d PD . .
Cl1B Cl -0.2409(4) -0.0305(3) 0.0134(8) 0.1082(12) Uani 0.37 1 d PD . .
C200 C 0.0000 0.0000 0.035(3) 0.140(18) Uani 0.50 3 d SP . .
H20A H 0.0000 0.0000 0.1162 0.168 Uiso 0.50 3 d SPR . .
Cl20 Cl 0.0500(3) -0.0085(4) 0.0017(5) 0.119(2) Uani 0.50 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 0.0033 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'
Cl Cl 0.1484 0.1585 '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 98.44(13) 17_444 18_554 ?
O1 Fe1 O7 74.80(13) 17_444 . ?
O7 Fe1 O7 98.88(18) 18_554 . ?
O1 Fe1 O1 167.37(16) 17_444 . ?
O7 Fe1 O1 74.38(13) 18_554 . ?
O7 Fe1 O1 95.76(13) . . ?
O1 Fe1 N10 92.33(12) 17_444 . ?
O7 Fe1 N10 97.96(13) 18_554 . ?
O7 Fe1 N10 160.11(13) . . ?
O1 Fe1 N10 98.90(13) . . ?
O1 Fe1 N4 107.84(14) 17_444 . ?
O7 Fe1 N4 151.81(13) 18_554 . ?
O7 Fe1 N4 78.88(13) . . ?
O1 Fe1 N4 77.88(13) . . ?
N10 Fe1 N4 91.11(13) . . ?
C2 O1 Fe1 133.8(3) . 18_554 ?
C2 O1 Fe1 120.7(3) . . ?
Fe1 O1 Fe1 105.35(14) 18_554 . ?
O1 C2 C3 107.7(4) . . ?
N4 C3 C2 109.8(3) . . ?
C8 N4 C5 110.5(4) . . ?
C8 N4 C3 111.1(3) . . ?
C5 N4 C3 113.3(4) . . ?
C8 N4 Fe1 111.7(3) . . ?
C5 N4 Fe1 107.4(3) . . ?
C3 N4 Fe1 102.7(3) . . ?
N4 C5 C6 111.7(4) . . ?
O7 C6 C5 109.7(4) . . ?
C6 O7 Fe1 128.4(3) . 17_444 ?
C6 O7 Fe1 113.8(2) . . ?
Fe1 O7 Fe1 105.33(14) 17_444 . ?
N4 C8 C9 114.9(4) . . ?
O10 C9 C8 107.2(4) . . ?
C11 O10 C9 117.9(5) . . ?
O10 C11 C12 125.0(6) . . ?
O10 C11 C16 114.6(6) . . ?
C12 C11 C16 120.4(6) . . ?
C11 C12 C13 117.1(8) . . ?
C14 C13 C12 121.4(8) . . ?
C15 C14 C13 120.7(8) . . ?
C14 C15 C16 121.4(10) . . ?
C15 C16 C11 118.8(8) . . ?
C10 N10 Fe1 160.6(5) . . ?
N10 C10 S10 174.4(6) . . ?
Cl11 C100 Cl1B 143.6(8) . . ?
Cl11 C100 Cl1A 32.5(4) . . ?
Cl1B C100 Cl1A 111.1(7) . . ?
Cl11 C100 Cl12 111.2(6) . . ?
Cl1B C100 Cl12 32.4(4) . . ?
Cl1A C100 Cl12 78.8(5) . . ?
Cl1A Cl11 C100 78.1(6) . . ?
Cl11 Cl1A C100 69.4(7) . . ?
Cl11 Cl1A Cl12 120.2(7) . . ?
C100 Cl1A Cl12 51.1(4) . . ?
Cl1B Cl12 C100 68.7(6) . . ?
Cl1B Cl12 Cl1A 118.6(7) . . ?
C100 Cl12 Cl1A 50.1(4) . . ?
Cl12 Cl1B C100 78.9(7) . . ?
C200 C200 Cl20 75.9(14) 10 2 ?
C200 C200 Cl20 75.9(14) 10 3 ?
Cl20 C200 Cl20 114.3(11) 2 3 ?
C200 C200 Cl20 75.9(14) 10 . ?
Cl20 C200 Cl20 114.3(11) 2 . ?
Cl20 C200 Cl20 114.3(11) 3 . ?
C200 C200 Cl20 74.6(14) 10 10 ?
Cl20 C200 Cl20 57.9(4) 2 10 ?
Cl20 C200 Cl20 57.9(4) 3 10 ?
Cl20 C200 Cl20 151(3) . 10 ?
C200 C200 Cl20 74.6(14) 10 12 ?
Cl20 C200 Cl20 57.9(4) 2 12 ?
Cl20 C200 Cl20 151(3) 3 12 ?
Cl20 C200 Cl20 57.9(4) . 12 ?
Cl20 C200 Cl20 113.2(12) 10 12 ?
C200 C200 Cl20 74.6(14) 10 11 ?
Cl20 C200 Cl20 151(3) 2 11 ?
Cl20 C200 Cl20 57.9(4) 3 11 ?
Cl20 C200 Cl20 57.9(4) . 11 ?
Cl20 C200 Cl20 113.2(12) 10 11 ?
Cl20 C200 Cl20 113.2(12) 12 11 ?
Cl20 Cl20 Cl20 119.94(4) 12 11 ?
Cl20 Cl20 C200 61.4(3) 12 . ?
Cl20 Cl20 C200 61.4(3) 11 . ?
Cl20 Cl20 C200 60.8(2) 12 10 ?
Cl20 Cl20 C200 60.8(2) 11 10 ?
C200 Cl20 C200 29(3) . 10 ?
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 1.974(3) 17_444 ?
Fe1 O7 1.984(3) 18_554 ?
Fe1 O7 2.002(3) . ?
Fe1 O1 2.012(3) . ?
Fe1 N10 2.145(4) . ?
Fe1 N4 2.278(4) . ?
O1 C2 1.427(5) . ?
O1 Fe1 1.974(3) 18_554 ?
C2 C3 1.528(6) . ?
C3 N4 1.498(6) . ?
N4 C8 1.492(6) . ?
N4 C5 1.496(6) . ?
C5 C6 1.526(6) . ?
C6 O7 1.417(5) . ?
O7 Fe1 1.984(3) 17_444 ?
C8 C9 1.529(7) . ?
C9 O10 1.444(7) . ?
O10 C11 1.362(7) . ?
C11 C12 1.378(9) . ?
C11 C16 1.411(11) . ?
C12 C13 1.436(10) . ?
C13 C14 1.363(14) . ?
C14 C15 1.319(14) . ?
C15 C16 1.404(11) . ?
N10 C10 0.989(9) . ?
S10 C10 1.682(9) . ?
C100 Cl11 1.686(9) . ?
C100 Cl1B 1.697(10) . ?
C100 Cl1A 1.762(11) . ?
C100 Cl12 1.788(10) . ?
Cl11 Cl1A 0.968(10) . ?
Cl1A Cl12 2.254(10) . ?
Cl12 Cl1B 0.977(11) . ?
C200 C200 0.84(8) 10 ?
C200 Cl20 1.639(11) 2 ?
C200 Cl20 1.639(11) 3 ?
C200 Cl20 1.639(11) . ?
C200 Cl20 1.649(11) 10 ?
C200 Cl20 1.649(11) 12 ?
C200 Cl20 1.649(11) 11 ?
Cl20 Cl20 1.590(6) 12 ?
Cl20 Cl20 1.590(6) 11 ?
Cl20 C200 1.649(11) 10 ?
