#------------------------------------------------------------------------------
#$Date: 2017-07-11 15:10:40 +0300 (Tue, 11 Jul 2017) $
#$Revision: 198633 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/00/57/7005716.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_7005716
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                   13.4838(4)
_cell_length_b                   13.4838(4)
_cell_length_c                   9.3520(6)
_cell_measurement_reflns_used    8718
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.56
_cell_measurement_theta_min      2.79
_cell_volume                     1472.52(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      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.944
_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  0.0204
_diffrn_reflns_av_sigmaI/netI    0.0143
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16951
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.68
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.863
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_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         0.375
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2884
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0270
_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)+(0.0406P)²+0.4838P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0761
_reflns_number_gt                2642
_reflns_number_total             2884
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b704823h.txt
_cod_data_source_block           ctbe48nh4ltm
_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_cell_volume        1472.51(11)
_cod_original_sg_symbol_H-M      P-3
_cod_database_code               7005716
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
Fe Fe 0.6667 0.3333 0.14241(3) 0.01605(8) Uani 1 3 d S . .
Cl Cl 1.07463(3) 0.23610(2) 0.25628(3) 0.02667(9) Uani 1 1 d . . .
O1 O 0.96967(8) 0.12609(8) 0.25007(11) 0.0336(2) Uani 1 1 d . . .
O2 O 1.13238(9) 0.24429(9) 0.38878(11) 0.0372(2) Uani 1 1 d . . .
O3 O 1.04823(11) 0.32630(10) 0.24634(15) 0.0493(3) Uani 1 1 d . . .
O4 O 1.14706(10) 0.24117(10) 0.13991(12) 0.0450(3) Uani 1 1 d . . .
N N 0.6667 0.3333 -0.2190(2) 0.0308(4) Uani 1 3 d S . .
N1 N 0.78372(8) 0.31509(9) 0.03758(10) 0.02219(19) Uani 1 1 d . . .
N2 N 0.66584(8) 0.21237(8) 0.25911(10) 0.02076(19) Uani 1 1 d . . .
N3 N 0.74547(11) 0.10821(11) 0.30738(14) 0.0359(3) Uani 1 1 d . . .
H3B H 0.7906 0.0787 0.3011 0.043 Uiso 1 1 calc R . .
N1A N 1.0000 0.0000 0.0000 0.0276(5) Uani 1 6 d S . .
H1A1 H 0.960(6) 0.007(8) 0.047(4) 0.11(2) Uiso 0.67 1 d P . .
N2A N 1.0000 0.0000 0.5000 0.0248(5) Uani 1 6 d S . .
H2A1 H 0.970(9) 0.029(9) 0.461(5) 0.13(3) Uiso 0.67 1 d P . .
C1 C 0.77569(13) 0.33844(14) -0.22499(14) 0.0337(3) Uani 1 1 d . . .
H1A H 0.8204 0.3893 -0.3050 0.040 Uiso 1 1 calc R . .
H1B H 0.7625 0.2609 -0.2468 0.040 Uiso 1 1 calc R . .
C2 C 0.84772(11) 0.38155(12) -0.08795(13) 0.0299(3) Uani 1 1 d . . .
H2A H 0.9178 0.3760 -0.0991 0.036 Uiso 1 1 calc R . .
H2B H 0.8715 0.4631 -0.0730 0.036 Uiso 1 1 calc R . .
C3 C 0.81172(11) 0.24500(12) 0.09406(14) 0.0277(2) Uani 1 1 d . . .
H3A H 0.8708 0.2333 0.0574 0.033 Uiso 1 1 calc R . .
C4 C 0.74452(11) 0.18643(11) 0.21806(13) 0.0253(2) Uani 1 1 d . . .
C5 C 0.61451(11) 0.14817(11) 0.37856(14) 0.0291(3) Uani 1 1 d . . .
H5A H 0.5546 0.1487 0.4314 0.035 Uiso 1 1 calc R . .
C6 C 0.66381(14) 0.08316(13) 0.40911(17) 0.0377(3) Uani 1 1 d . . .
H6A H 0.6448 0.0308 0.4862 0.045 Uiso 1 1 calc R . .
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 91.95(4) 2_655 . ?
N2 Fe N2 91.95(4) 2_655 3_665 ?
N2 Fe N2 91.95(4) . 3_665 ?
N2 Fe N1 89.59(4) 2_655 . ?
N2 Fe N1 81.08(4) . . ?
N2 Fe N1 172.91(4) 3_665 . ?
N2 Fe N1 81.08(4) 2_655 2_655 ?
N2 Fe N1 172.91(4) . 2_655 ?
N2 Fe N1 89.58(4) 3_665 2_655 ?
N1 Fe N1 97.49(4) . 2_655 ?
N2 Fe N1 172.91(4) 2_655 3_665 ?
N2 Fe N1 89.59(4) . 3_665 ?
N2 Fe N1 81.08(4) 3_665 3_665 ?
N1 Fe N1 97.49(4) . 3_665 ?
N1 Fe N1 97.49(4) 2_655 3_665 ?
O3 Cl O2 110.24(7) . . ?
O3 Cl O4 111.19(8) . . ?
O2 Cl O4 108.60(7) . . ?
O3 Cl O1 109.64(7) . . ?
O2 Cl O1 109.07(6) . . ?
O4 Cl O1 108.04(7) . . ?
C1 N C1 119.849(13) . 3_665 ?
C1 N C1 119.848(13) . 2_655 ?
C1 N C1 119.844(13) 3_665 2_655 ?
C3 N1 C2 118.41(11) . . ?
C3 N1 Fe 115.59(8) . . ?
C2 N1 Fe 125.71(8) . . ?
C4 N2 C5 106.66(10) . . ?
C4 N2 Fe 112.67(8) . . ?
C5 N2 Fe 140.49(9) . . ?
C4 N3 C6 107.65(11) . . ?
C4 N3 H3B 126.2 . . ?
C6 N3 H3B 126.2 . . ?
N C1 C2 115.04(12) . . ?
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 111.65(11) . . ?
N1 C2 H2A 109.3 . . ?
C1 C2 H2A 109.3 . . ?
N1 C2 H2B 109.3 . . ?
C1 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
N1 C3 C4 113.34(11) . . ?
N1 C3 H3A 123.3 . . ?
C4 C3 H3A 123.3 . . ?
N2 C4 N3 110.33(12) . . ?
N2 C4 C3 117.03(11) . . ?
N3 C4 C3 132.63(12) . . ?
C6 C5 N2 108.72(12) . . ?
C6 C5 H5A 125.6 . . ?
N2 C5 H5A 125.6 . . ?
N3 C6 C5 106.63(12) . . ?
N3 C6 H6A 126.7 . . ?
C5 C6 H6A 126.7 . . ?
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 1.9578(10) 2_655 ?
Fe N2 1.9579(10) . ?
Fe N2 1.9579(10) 3_665 ?
Fe N1 1.9751(10) . ?
Fe N1 1.9751(10) 2_655 ?
Fe N1 1.9751(10) 3_665 ?
Cl O3 1.4308(11) . ?
Cl O2 1.4381(10) . ?
Cl O4 1.4409(11) . ?
Cl O1 1.4516(10) . ?
N C1 1.4379(15) . ?
N C1 1.4380(15) 3_665 ?
N C1 1.4380(15) 2_655 ?
N1 C3 1.2929(16) . ?
N1 C2 1.4672(15) . ?
N2 C4 1.3290(15) . ?
N2 C5 1.3701(16) . ?
N3 C4 1.3505(16) . ?
N3 C6 1.364(2) . ?
N3 H3B 0.8800 . ?
N1A H1A1 0.74(4) . ?
N2A H2A1 0.78(4) . ?
C1 C2 1.5360(19) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.4402(18) . ?
C3 H3A 0.9500 . ?
C5 C6 1.3692(19) . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9500 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3B O1 0.88 2.22 2.9589(16) 141.6 .
N3 H3B O2 0.88 2.51 3.1333(16) 128.6 2_645
N3 H3B O4 0.88 2.62 3.2278(18) 126.6 2_645
N1A H1A1 O1 0.74(4) 2.45(6) 3.0369(10) 138(7) .
N1A H1A1 O4 0.74(4) 2.50(6) 3.1258(12) 143(9) 2_645
N2A H2A1 O1 0.78(4) 2.37(6) 3.0359(11) 144(7) .
N2A H2A1 O2 0.78(4) 2.58(4) 3.0395(11) 119(4) 6_546
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 87.03(10) 2_655 . . . ?
N2 Fe N1 C3 -5.01(9) . . . . ?
N2 Fe N1 C3 -15.5(4) 3_665 . . . ?
N1 Fe N1 C3 167.98(9) 2_655 . . . ?
N1 Fe N1 C3 -93.40(11) 3_665 . . . ?
N2 Fe N1 C2 -86.65(10) 2_655 . . . ?
N2 Fe N1 C2 -178.69(10) . . . . ?
N2 Fe N1 C2 170.8(3) 3_665 . . . ?
N1 Fe N1 C2 -5.70(10) 2_655 . . . ?
N1 Fe N1 C2 92.92(8) 3_665 . . . ?
N2 Fe N2 C4 -85.10(10) 2_655 . . . ?
N2 Fe N2 C4 -177.12(8) 3_665 . . . ?
N1 Fe N2 C4 4.17(8) . . . . ?
N1 Fe N2 C4 -74.7(4) 2_655 . . . ?
N1 Fe N2 C4 101.82(9) 3_665 . . . ?
N2 Fe N2 C5 89.17(11) 2_655 . . . ?
N2 Fe N2 C5 -2.84(14) 3_665 . . . ?
N1 Fe N2 C5 178.45(14) . . . . ?
N1 Fe N2 C5 99.5(4) 2_655 . . . ?
N1 Fe N2 C5 -83.90(14) 3_665 . . . ?
C1 N C1 C2 -113.84(18) 3_665 . . . ?
C1 N C1 C2 74.0(2) 2_655 . . . ?
C3 N1 C2 C1 107.76(13) . . . . ?
Fe N1 C2 C1 -78.72(13) . . . . ?
N C1 C2 N1 54.26(16) . . . . ?
C2 N1 C3 C4 178.84(11) . . . . ?
Fe N1 C3 C4 4.67(14) . . . . ?
C5 N2 C4 N3 -0.20(14) . . . . ?
Fe N2 C4 N3 176.00(9) . . . . ?
C5 N2 C4 C3 -179.21(11) . . . . ?
Fe N2 C4 C3 -3.01(14) . . . . ?
C6 N3 C4 N2 0.19(16) . . . . ?
C6 N3 C4 C3 178.99(14) . . . . ?
N1 C3 C4 N2 -1.07(17) . . . . ?
N1 C3 C4 N3 -179.81(14) . . . . ?
C4 N2 C5 C6 0.14(15) . . . . ?
Fe N2 C5 C6 -174.35(11) . . . . ?
C4 N3 C6 C5 -0.09(17) . . . . ?
N2 C5 C6 N3 -0.03(17) . . . . ?
