#------------------------------------------------------------------------------
#$Date: 2017-07-11 15:10:40 +0300 (Tue, 11 Jul 2017) $
#$Revision: 198633 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/00/57/7005714.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_7005714
loop_
_publ_author_name
'Brewer, Greg'
'Butcher, Ray J.'
'Viragh, Carol'
'White, Genevieve'
_publ_section_title
;
 Supramolecular assemblies prepared from an iron(II) tripodal imidazole
 complex. A molecular scaffolding for the self assembly of icosahedral
 complexes of K+, Rb+, Cs+ and NH4+ cations
;
_journal_issue                   37
_journal_name_full               'Dalton Transactions'
_journal_page_first              4132
_journal_paper_doi               10.1039/b704823h
_journal_year                    2007
_chemical_formula_sum            'C18 H28 Cl3 Fe N11 O12'
_chemical_formula_weight         752.71
_chemical_name_systematic        ?
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_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                   13.5873(4)
_cell_length_b                   13.5873(4)
_cell_length_c                   9.3764(6)
_cell_measurement_reflns_used    9979
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.58
_cell_measurement_theta_min      2.78
_cell_volume                     1499.11(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0151
_diffrn_reflns_av_sigmaI/netI    0.0093
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17231
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.64
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.848
_exptl_absorpt_correction_T_max  0.9200
_exptl_absorpt_correction_T_min  0.7067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         2929
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0592P)²+0.4344P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0967
_refine_ls_wR_factor_ref         0.0999
_reflns_number_gt                2696
_reflns_number_total             2929
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b704823h.txt
_cod_data_source_block           ctbe48nh4m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' 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 

The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'constrained' was replaced with
the value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_sg_symbol_H-M      P-3
_cod_database_code               7005714
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'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
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Fe Fe 1.3333 0.6667 1.13841(3) 0.02756(10) Uani 1 3 d S . . 0
Cl Cl 0.92608(3) 0.16307(3) 1.25572(4) 0.04692(12) Uani 1 1 d . . . 0
O1 O 0.95312(17) 0.27832(14) 1.2474(2) 0.0892(6) Uani 1 1 d . . . 0
O2 O 0.86689(14) 0.11242(14) 1.38543(17) 0.0690(4) Uani 1 1 d . . . 0
O3 O 0.85484(16) 0.09534(18) 1.13967(18) 0.0819(5) Uani 1 1 d . . . 0
O4 O 1.02903(11) 0.15640(12) 1.25098(16) 0.0586(3) Uani 1 1 d . . . 0
N1A N 1.0000 0.0000 1.0000 0.0467(7) Uani 1 6 d S . . 4
N2A N 1.0000 0.0000 1.5000 0.0430(6) Uani 1 6 d S . . 4
N N 1.3333 0.6667 0.7792(3) 0.0533(6) Uani 1 3 d S . . 0
N1 N 1.21600(10) 0.53289(10) 1.03395(12) 0.0373(2) Uani 1 1 d . . . 0
N2 N 1.33254(10) 0.54618(10) 1.25446(12) 0.0350(2) Uani 1 1 d . . . 0
N3 N 1.25334(16) 0.36415(13) 1.30107(19) 0.0608(4) Uani 1 1 d . . . 0
H3B H 1.2092 0.2918 1.2944 0.073 Uiso 1 1 calc R . . 0
C1 C 1.22465(17) 0.56441(18) 0.77249(17) 0.0567(4) Uani 1 1 d . . . 0
H1A H 1.2367 0.5014 0.7509 0.068 Uiso 1 1 calc R . . 0
H1B H 1.1817 0.5712 0.6943 0.068 Uiso 1 1 calc R . . 0
C2 C 1.15313(14) 0.53614(16) 0.90873(17) 0.0502(4) Uani 1 1 d . . . 0
H2A H 1.1307 0.5929 0.9233 0.060 Uiso 1 1 calc R . . 0
H2B H 1.0846 0.4629 0.8976 0.060 Uiso 1 1 calc R . . 0
C3 C 1.18766(14) 0.43560(13) 1.09010(17) 0.0462(3) Uani 1 1 d . . . 0
H3A H 1.1298 0.3671 1.0543 0.055 Uiso 1 1 calc R . . 0
C4 C 1.25404(14) 0.44309(12) 1.21317(17) 0.0427(3) Uani 1 1 d . . . 0
C5 C 1.38350(15) 0.53230(15) 1.37261(18) 0.0491(4) Uani 1 1 d . . . 0
H5A H 1.4420 0.5904 1.4247 0.059 Uiso 1 1 calc R . . 0
C6 C 1.3339(2) 0.41844(18) 1.4012(2) 0.0643(5) Uani 1 1 d . . . 0
H6A H 1.3522 0.3851 1.4754 0.077 Uiso 1 1 calc R . . 0
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
N2 Fe N2 92.19(5) 3_775 . ?
N2 Fe N2 92.20(5) 3_775 2_755 ?
N2 Fe N2 92.19(5) . 2_755 ?
N2 Fe N1 172.97(5) 3_775 2_755 ?
N2 Fe N1 89.44(5) . 2_755 ?
N2 Fe N1 80.91(5) 2_755 2_755 ?
N2 Fe N1 80.91(5) 3_775 3_775 ?
N2 Fe N1 172.98(5) . 3_775 ?
N2 Fe N1 89.44(5) 2_755 3_775 ?
N1 Fe N1 97.57(5) 2_755 3_775 ?
N2 Fe N1 89.44(5) 3_775 . ?
N2 Fe N1 80.91(5) . . ?
N2 Fe N1 172.97(5) 2_755 . ?
N1 Fe N1 97.57(5) 2_755 . ?
N1 Fe N1 97.57(5) 3_775 . ?
O1 Cl O2 110.49(11) . . ?
O1 Cl O3 112.55(13) . . ?
O2 Cl O3 107.35(12) . . ?
O1 Cl O4 110.01(10) . . ?
O2 Cl O4 108.94(9) . . ?
O3 Cl O4 107.37(10) . . ?
C1 N C1 119.812(19) 3_775 . ?
C1 N C1 119.81(2) 3_775 2_755 ?
C1 N C1 119.808(19) . 2_755 ?
C3 N1 C2 118.55(13) . . ?
C3 N1 Fe 115.49(10) . . ?
C2 N1 Fe 125.70(11) . . ?
C4 N2 C5 106.62(13) . . ?
C4 N2 Fe 112.70(10) . . ?
C5 N2 Fe 140.55(11) . . ?
C6 N3 C4 108.03(15) . . ?
C6 N3 H3B 126.0 . . ?
C4 N3 H3B 126.0 . . ?
N C1 C2 114.97(16) . . ?
N C1 H1A 108.5 . . ?
C2 C1 H1A 108.5 . . ?
N C1 H1B 108.5 . . ?
C2 C1 H1B 108.5 . . ?
H1A C1 H1B 107.5 . . ?
N1 C2 C1 111.66(14) . . ?
N1 C2 H2A 109.3 . . ?
C1 C2 H2A 109.3 . . ?
N1 C2 H2B 109.3 . . ?
C1 C2 H2B 109.3 . . ?
H2A C2 H2B 107.9 . . ?
N1 C3 C4 113.58(13) . . ?
N1 C3 H3A 123.2 . . ?
C4 C3 H3A 123.2 . . ?
N2 C4 N3 110.12(15) . . ?
N2 C4 C3 117.04(13) . . ?
N3 C4 C3 132.84(15) . . ?
N2 C5 C6 108.48(17) . . ?
N2 C5 H5A 125.8 . . ?
C6 C5 H5A 125.8 . . ?
N3 C6 C5 106.74(16) . . ?
N3 C6 H6A 126.6 . . ?
C5 C6 H6A 126.6 . . ?
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
Fe N2 1.9611(11) 3_775 ?
Fe N2 1.9612(11) . ?
Fe N2 1.9612(11) 2_755 ?
Fe N1 1.9766(12) 2_755 ?
Fe N1 1.9766(12) 3_775 ?
Fe N1 1.9766(12) . ?
Cl O1 1.4206(16) . ?
Cl O2 1.4305(15) . ?
Cl O3 1.4412(17) . ?
Cl O4 1.4469(13) . ?
N C1 1.436(2) 3_775 ?
N C1 1.436(2) . ?
N C1 1.437(2) 2_755 ?
N1 C3 1.290(2) . ?
N1 C2 1.466(2) . ?
N2 C4 1.3249(19) . ?
N2 C5 1.3686(19) . ?
N3 C6 1.348(3) . ?
N3 C4 1.349(2) . ?
N3 H3B 0.8600 . ?
C1 C2 1.533(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.437(2) . ?
C3 H3A 0.9300 . ?
C5 C6 1.370(3) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?
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
N2 Fe N1 C3 -87.46(12) 3_775 . . . ?
N2 Fe N1 C3 4.85(12) . . . . ?
N2 Fe N1 C3 16.1(5) 2_755 . . . ?
N1 Fe N1 C3 93.06(14) 2_755 . . . ?
N1 Fe N1 C3 -168.21(12) 3_775 . . . ?
N2 Fe N1 C2 86.66(13) 3_775 . . . ?
N2 Fe N1 C2 178.97(13) . . . . ?
N2 Fe N1 C2 -169.8(4) 2_755 . . . ?
N1 Fe N1 C2 -92.82(10) 2_755 . . . ?
N1 Fe N1 C2 5.90(13) 3_775 . . . ?
N2 Fe N2 C4 85.13(13) 3_775 . . . ?
N2 Fe N2 C4 177.41(10) 2_755 . . . ?
N1 Fe N2 C4 -101.71(11) 2_755 . . . ?
N1 Fe N2 C4 74.1(4) 3_775 . . . ?
N1 Fe N2 C4 -3.95(10) . . . . ?
N2 Fe N2 C5 -90.01(15) 3_775 . . . ?
N2 Fe N2 C5 2.27(17) 2_755 . . . ?
N1 Fe N2 C5 83.15(17) 2_755 . . . ?
N1 Fe N2 C5 -101.1(4) 3_775 . . . ?
N1 Fe N2 C5 -179.09(18) . . . . ?
C1 N C1 C2 -74.5(3) 3_775 . . . ?
C1 N C1 C2 114.2(2) 2_755 . . . ?
C3 N1 C2 C1 -107.64(18) . . . . ?
Fe N1 C2 C1 78.41(18) . . . . ?
N C1 C2 N1 -54.1(2) . . . . ?
C2 N1 C3 C4 -179.20(14) . . . . ?
Fe N1 C3 C4 -4.64(18) . . . . ?
C5 N2 C4 N3 0.02(19) . . . . ?
Fe N2 C4 N3 -176.76(12) . . . . ?
C5 N2 C4 C3 179.53(14) . . . . ?
Fe N2 C4 C3 2.75(18) . . . . ?
C6 N3 C4 N2 -0.1(2) . . . . ?
C6 N3 C4 C3 -179.51(19) . . . . ?
N1 C3 C4 N2 1.2(2) . . . . ?
N1 C3 C4 N3 -179.40(18) . . . . ?
C4 N2 C5 C6 0.1(2) . . . . ?
Fe N2 C5 C6 175.40(14) . . . . ?
C4 N3 C6 C5 0.1(2) . . . . ?
N2 C5 C6 N3 -0.1(2) . . . . ?
