#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2008541.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2008541
loop_
_publ_author_name
'Alcock, N. W.'
'Zhang, D.'
'Busch, D. H.'
_publ_section_title
;
 Tris(2-pyridylmethyl)triazacyclododecane complexes of Fe^II^ and
 Cu^II^
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              886
_journal_page_last               889
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          '[Fe (C27 H36 N6)] [Fe Cl4]'
_chemical_formula_sum            'C27 H36 Cl4 Fe2 N6'
_chemical_formula_weight         698.12
_chemical_name_systematic
;
;
_space_group_IT_number           205
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.793(2)
_cell_length_b                   18.793(2)
_cell_length_c                   18.793(2)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      10
_cell_volume                     6637.3(12)
_computing_cell_refinement       R3M
_computing_data_collection       'R3M (Siemens, 1986)'
_computing_data_reduction        R3M
_computing_molecular_graphics    'XP (Siemens, 1995)'
_computing_publication_material  'XCIF (Siemens, 1995)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL-Plus (Sheldrick, 1990a)'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       'Siemens R3m'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Normal focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.127
_diffrn_reflns_av_sigmaI/netI    0.0973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       1
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2262
_diffrn_reflns_theta_max         22.54
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        22
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.223
_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   '(SHELXTL-Plus; Sheldrick, 1990a)'
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.37
_refine_diff_density_max         0.758
_refine_diff_density_min         -0.377
_refine_ls_extinction_coef       0.0012(4)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_all   1.094
_refine_ls_goodness_of_fit_obs   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         1461
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.092
_refine_ls_restrained_S_obs      1.161
_refine_ls_R_factor_all          0.088
_refine_ls_R_factor_obs          0.063
_refine_ls_shift/esd_max         <0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w = 1/[\s^2^(Fo^2^)+(0.0720P)^2^+17.7800P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_all         0.173
_refine_ls_wR_factor_obs         0.157
_reflns_number_observed          1098
_reflns_number_total             1461
_reflns_observed_criterion       I>2\s(I)
_[local]_cod_data_source_file    cf1275.cif
_[local]_cod_data_source_block   delcub
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

'_geom_bond_publ_flag'
value 'Y' changed to 'y' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (2
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (5 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        6637.3(13)
_cod_database_code               2008541
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-z, -x, -y'
'-z-1/2, x-1/2, y'
'z-1/2, x, -y-1/2'
'z, -x-1/2, y-1/2'
'-y, -z, -x'
'y, -z-1/2, x-1/2'
'-y-1/2, z-1/2, x'
'y-1/2, z, -x-1/2'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Fe1 0.0270(5) 0.0270(5) 0.0270(5) 0.0004(4) 0.0004(4) 0.0004(4)
Fe2 0.0337(6) 0.0337(6) 0.0337(6) 0.0037(5) 0.0037(5) 0.0037(5)
Cl1 0.0388(8) 0.0388(8) 0.0388(8) 0.0026(8) 0.0026(8) 0.0026(8)
Cl2 0.0723(15) 0.0367(12) 0.0567(13) -0.0089(10) -0.0066(11) 0.0132(9)
N1 0.032(3) 0.028(3) 0.034(3) 0.000(3) 0.008(3) -0.002(3)
N2 0.029(3) 0.028(3) 0.038(3) -0.001(3) 0.001(3) -0.002(3)
C1 0.028(4) 0.061(5) 0.050(5) -0.008(4) 0.004(4) 0.004(4)
C2A 0.038(7) 0.067(10) 0.049(8) -0.010(6) -0.013(5) 0.008(7)
C2B 0.021(12) 0.058(18) 0.035(14) 0.002(11) -0.016(10) 0.007(12)
C3 0.030(4) 0.046(4) 0.053(5) 0.001(3) -0.012(4) 0.005(4)
C4 0.044(4) 0.037(4) 0.039(4) -0.001(4) 0.010(4) 0.000(3)
C5 0.034(4) 0.033(4) 0.031(4) -0.004(3) 0.002(3) 0.001(3)
C6 0.045(4) 0.037(4) 0.045(4) -0.002(4) 0.012(4) -0.009(4)
C7 0.056(5) 0.032(4) 0.051(5) 0.004(4) 0.010(4) -0.013(4)
C8 0.050(5) 0.028(4) 0.040(4) 0.004(4) -0.001(4) 0.001(3)
C9 0.041(4) 0.033(4) 0.044(5) -0.001(3) 0.007(4) 0.007(4)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_group
_atom_site_type_symbol
Fe1 0.63084(5) 0.63084(5) 0.63084(5) 0.0270(5) Uani d S 1 . Fe
Fe2 0.16689(5) 0.16689(5) 0.16689(5) 0.0337(6) Uani d S 1 . Fe
Cl1 0.09424(10) 0.09424(10) 0.09424(10) 0.0388(8) Uani d S 1 . Cl
Cl2 0.17626(12) 0.27680(10) 0.11202(11) 0.0553(7) Uani d . 1 . Cl
N1 0.7405(3) 0.6632(3) 0.5942(3) 0.0312(14) Uani d . 1 . N
N2 0.6671(3) 0.5365(3) 0.5690(3) 0.0317(14) Uani d . 1 . N
C1 0.8001(4) 0.6358(4) 0.6409(4) 0.046(2) Uani d . 1 . C
H1A 0.8091 0.5857 0.6276 0.056 Uiso calc PR 0.687(17) 1 H
H1B 0.8436 0.6631 0.6290 0.056 Uiso calc PR 0.687(17) 1 H
H1C 0.8180 0.6760 0.6699 0.056 Uiso calc PR 0.313(17) 2 H
H1D 0.8396 0.6204 0.6096 0.056 Uiso calc PR 0.313(17) 2 H
C2A 0.7907(6) 0.6387(7) 0.7181(6) 0.051(4) Uani d P 0.687(17) 1 C
H2AA 0.7723 0.6864 0.7307 0.062 Uiso calc PR 0.687(17) 1 H
H2AB 0.8381 0.6336 0.7407 0.062 Uiso calc PR 0.687(17) 1 H
C2B 0.7819(11) 0.5732(14) 0.6921(12) 0.038(8) Uani d PU 0.313(17) 2 C
H2BA 0.7585 0.5360 0.6630 0.046 Uiso calc PR 0.313(17) 2 H
H2BB 0.8277 0.5530 0.7085 0.046 Uiso calc PR 0.313(17) 2 H
C3 0.7409(4) 0.5828(4) 0.7508(4) 0.0430(19) Uani d . 1 . C
H3A 0.7534 0.5359 0.7305 0.052 Uiso calc PR 0.687(17) 1 H
H3B 0.7504 0.5806 0.8025 0.052 Uiso calc PR 0.687(17) 1 H
H3C 0.7599 0.6243 0.7771 0.052 Uiso calc PR 0.313(17) 2 H
H3D 0.7470 0.5407 0.7818 0.052 Uiso calc PR 0.313(17) 2 H
C4 0.7478(4) 0.6272(3) 0.5229(4) 0.0402(18) Uani d . 1 . C
H4A 0.7984 0.6278 0.5082 0.048 Uiso calc R 1 . H
H4B 0.7202 0.6541 0.4870 0.048 Uiso calc R 1 . H
C5 0.7218(3) 0.5511(4) 0.5246(3) 0.0325(17) Uani d . 1 . C
C6 0.7508(4) 0.4997(4) 0.4796(4) 0.0421(18) Uani d . 1 . C
H6A 0.7903 0.5106 0.4499 0.051 Uiso calc R 1 . H
C7 0.7209(4) 0.4324(4) 0.4791(4) 0.046(2) Uani d . 1 . C
H7A 0.7391 0.3966 0.4484 0.055 Uiso calc R 1 . H
C8 0.6643(4) 0.4176(4) 0.5236(4) 0.0396(18) Uani d . 1 . C
H8A 0.6434 0.3716 0.5241 0.047 Uiso calc R 1 . H
C9 0.6390(4) 0.4699(4) 0.5668(4) 0.0393(18) Uani d . 1 . C
H9A 0.5998 0.4594 0.5969 0.047 Uiso calc R 1 . H
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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 Fe1 N2 9 5 89.3(2) ?
N2 Fe1 N2 9 . 89.3(2) y
N2 Fe1 N2 5 . 89.3(2) ?
N2 Fe1 N1 9 . 164.0(2) y
N2 Fe1 N1 5 . 98.7(2) ?
N2 Fe1 N1 . . 77.04(19) y
N2 Fe1 N1 9 9 77.04(19) ?
N2 Fe1 N1 5 9 164.0(2) ?
N2 Fe1 N1 . 9 98.7(2) y
N1 Fe1 N1 . 9 96.57(18) y
N2 Fe1 N1 9 5 98.7(2) ?
N2 Fe1 N1 5 5 77.04(19) ?
N2 Fe1 N1 . 5 164.0(2) ?
N1 Fe1 N1 . 5 96.57(18) ?
N1 Fe1 N1 9 5 96.57(18) ?
Cl2 Fe2 Cl2 . 9 111.31(6) ?
Cl2 Fe2 Cl2 . 5 111.31(6) ?
Cl2 Fe2 Cl2 9 5 111.31(6) ?
Cl2 Fe2 Cl1 . . 107.57(6) ?
Cl2 Fe2 Cl1 9 . 107.57(6) ?
Cl2 Fe2 Cl1 5 . 107.57(6) ?
C3 N1 C4 5 . 107.5(5) ?
C3 N1 C1 5 . 108.7(5) ?
C4 N1 C1 . . 107.2(5) ?
C3 N1 Fe1 5 . 115.3(4) ?
C4 N1 Fe1 . . 103.5(4) ?
C1 N1 Fe1 . . 114.1(4) ?
C5 N2 C9 . . 117.5(6) ?
C5 N2 Fe1 . . 113.2(4) ?
C9 N2 Fe1 . . 129.1(5) ?
C2A C1 N1 . . 118.2(7) ?
N1 C1 C2B . . 116.8(9) ?
C1 C2A C3 . . 116.4(9) ?
C3 C2B C1 . . 121.7(18) ?
C2B C3 N1 . 9 118.1(10) ?
N1 C3 C2A 9 . 116.6(7) ?
N1 C4 C5 . . 112.1(6) ?
N2 C5 C6 . . 122.1(6) ?
N2 C5 C4 . . 116.8(6) ?
C6 C5 C4 . . 121.0(6) ?
C7 C6 C5 . . 118.6(7) ?
C8 C7 C6 . . 119.5(7) ?
C9 C8 C7 . . 119.0(7) ?
N2 C9 C8 . . 123.3(7) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 N2 9 2.226(5) ?
Fe1 N2 5 2.226(5) ?
Fe1 N2 . 2.226(5) y
Fe1 N1 . 2.257(5) y
Fe1 N1 9 2.257(5) ?
Fe1 N1 5 2.257(5) ?
Fe2 Cl2 . 2.3154(19) ?
Fe2 Cl2 9 2.3155(19) ?
Fe2 Cl2 5 2.3155(19) ?
Fe2 Cl1 . 2.365(4) ?
N1 C3 5 1.488(8) ?
N1 C4 . 1.509(9) ?
N1 C1 . 1.512(9) ?
N2 C5 . 1.352(8) ?
N2 C9 . 1.359(9) ?
C1 C2A . 1.464(14) ?
C1 C2B . 1.56(2) ?
C2A C3 . 1.535(13) ?
C2B C3 . 1.36(2) ?
C3 N1 9 1.488(8) ?
C4 C5 . 1.511(9) ?
C5 C6 . 1.395(10) ?
C6 C7 . 1.384(10) ?
C7 C8 . 1.381(10) ?
C8 C9 . 1.361(10) ?