#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:39:42 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179801 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/97/7009741.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_7009741
loop_
_publ_author_name
'Kou, Hui-Zhong'
'Bu, Wei-Ming'
'Gao, Song'
'Liao, Dai-Zheng'
'Jiang, Zong-Hui'
'Yan, Shi-Ping'
'Fan, Yu-Guo'
'Wang, Geng-Lin'
_publ_section_title
;
 Reactions between macrocyclic nickel(II) complexes and ferricyanide.
 Metamagnetic properties of a two-dimensional honeycomb assembly
 [NiL3]3[Fe(CN)6]2·8H2O
 (L3 = 3,10-dihydroxyethyl-1,3,6,8,10,12-hexaazacyclotetradecane) †
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2996
_journal_paper_doi               10.1039/b003289l
_journal_year                    2000
_chemical_formula_sum            'C48 H106 Fe2 N30 Ni3 O14'
_chemical_formula_weight         1615.33
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           165
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   14.993(3)
_cell_length_b                   14.993(3)
_cell_length_c                   18.450(3)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.35
_cell_measurement_theta_min      4.72
_cell_volume                     3591.7(12)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω 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  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            4951
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.57
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.239
_exptl_absorpt_correction_T_max  0.9534
_exptl_absorpt_correction_T_min  0.7332
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'red brown'
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       hexagon
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       0.0007(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.169
_refine_ls_goodness_of_fit_obs   1.455
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.169
_refine_ls_restrained_S_obs      1.455
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_obs          0.0456
_refine_ls_shift/esd_max         0.009
_refine_ls_shift/esd_mean        0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0732P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0721
_refine_ls_wR_factor_obs         0.0652
_reflns_number_observed          1875
_reflns_number_total             2113
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b003289l.txt
_cod_data_source_block           3
_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_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0732P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0732P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3591.8(12)
_cod_original_sg_symbol_H-M      P-3c1
_cod_database_code               7009741
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ni Ni 0.0000 0.5000 0.0000 0.0334(4) Uani 1 d S .
Fe Fe 0.3333 0.6667 -0.14944(10) 0.0308(5) Uani 1 d S .
O1 O 0.1067(8) 0.1934(8) 0.1254(6) 0.038(4) Uani 1 d . .
H1 H 0.0777(8) 0.1425(8) 0.0992(6) 0.207 Uiso 1 calc R .
N1 N 0.1423(5) 0.5871(5) -0.0505(4) 0.037(2) Uani 1 d . .
N2 N 0.2266(8) 0.4623(7) -0.2343(4) 0.081(3) Uani 1 d . .
N3 N -0.0207(5) 0.3657(5) -0.0517(4) 0.040(2) Uani 1 d . .
H3 H -0.0565(5) 0.3686(5) -0.0163(4) 0.048 Uiso 1 calc R .
N4 N -0.0683(5) 0.5201(5) -0.0917(4) 0.041(2) Uani 1 d . .
H4 H -0.0035(5) 0.5531(5) -0.0821(4) 0.049 Uiso 1 calc R .
N5 N 0.0910(5) 0.3434(6) 0.0342(4) 0.043(2) Uani 1 d . .
C1 C 0.2127(6) 0.6179(6) -0.0879(4) 0.033(2) Uani 1 d . .
C2 C 0.2650(8) 0.5411(7) -0.2056(4) 0.049(2) Uani 1 d . .
C3 C -0.0437(8) 0.3781(8) -0.1274(5) 0.057(3) Uani 1 d . .
H3A H -0.0740(8) 0.3125(8) -0.1524(5) 0.068 Uiso 1 calc R .
H3B H 0.0192(8) 0.4262(8) -0.1524(5) 0.068 Uiso 1 calc R .
C4 C -0.1194(7) 0.4191(7) -0.1271(5) 0.054(3) Uani 1 d . .
H4A H -0.1383(7) 0.4253(7) -0.1764(5) 0.065 Uiso 1 calc R .
H4B H -0.1816(7) 0.3721(7) -0.1009(5) 0.065 Uiso 1 calc R .
C5 C 0.0664(7) 0.3480(7) -0.0392(5) 0.048(3) Uani 1 d . .
H5A H 0.0510(7) 0.2839(7) -0.0625(5) 0.058 Uiso 1 calc R .
H5B H 0.1269(7) 0.4028(7) -0.0628(5) 0.058 Uiso 1 calc R .
C6 C 0.1379(7) 0.4393(7) 0.0739(5) 0.049(3) Uani 1 d . .
H6A H 0.1951(7) 0.4907(7) 0.0456(5) 0.058 Uiso 1 calc R .
H6B H 0.1659(7) 0.4298(7) 0.1187(5) 0.058 Uiso 1 calc R .
C7 C 0.0094(9) 0.2548(7) 0.0730(6) 0.070(3) Uani 1 d . .
H7A H -0.0161(9) 0.1952(7) 0.0415(6) 0.084 Uiso 1 calc R .
H7B H -0.0470(9) 0.2679(7) 0.0810(6) 0.084 Uiso 1 calc R .
C8 C 0.0369(13) 0.2280(14) 0.1435(10) 0.058(7) Uani 1 d . .
H8A H 0.0694(13) 0.2878(14) 0.1750(10) 0.190 Uiso 1 calc R .
H8B H -0.0236(13) 0.1741(14) 0.1675(10) 0.190 Uiso 1 calc R .
OW1 O 0.0000 0.0000 0.0674(10) 0.138(6) Uani 1 d S .
OW2 O 0.0000 0.3993(11) 0.2500 0.185(7) Uani 1 d S .
OW3 O -0.1873(16) 0.0540(16) 0.2374(13) 0.147(10) Uani 0.50 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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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
N4 Ni N4 180.0 7_565 . ?
N4 Ni N1 88.2(3) 7_565 7_565 ?
N4 Ni N1 91.8(3) . 7_565 ?
N4 Ni N1 91.8(3) 7_565 . ?
N4 Ni N1 88.2(3) . . ?
N1 Ni N1 180.0 7_565 . ?
N4 Ni N3 85.6(3) 7_565 7_565 ?
N4 Ni N3 94.4(3) . 7_565 ?
N1 Ni N3 90.7(3) 7_565 7_565 ?
N1 Ni N3 89.3(3) . 7_565 ?
N4 Ni N3 94.4(3) 7_565 . ?
N4 Ni N3 85.6(3) . . ?
N1 Ni N3 89.3(3) 7_565 . ?
N1 Ni N3 90.7(3) . . ?
N3 Ni N3 180.0 7_565 . ?
C2 Fe C2 94.0(3) 3_565 . ?
C2 Fe C2 94.0(3) 3_565 2_665 ?
C2 Fe C2 94.0(3) . 2_665 ?
C2 Fe C1 86.3(4) 3_565 . ?
C2 Fe C1 90.4(4) . . ?
C2 Fe C1 175.6(4) 2_665 . ?
C2 Fe C1 90.4(4) 3_565 3_565 ?
C2 Fe C1 175.6(4) . 3_565 ?
C2 Fe C1 86.3(4) 2_665 3_565 ?
C1 Fe C1 89.3(3) . 3_565 ?
C2 Fe C1 175.6(4) 3_565 2_665 ?
C2 Fe C1 86.3(4) . 2_665 ?
C2 Fe C1 90.4(4) 2_665 2_665 ?
C1 Fe C1 89.3(3) . 2_665 ?
C1 Fe C1 89.3(3) 3_565 2_665 ?
C1 N1 Ni 165.7(7) . . ?
C3 N3 C5 117.1(7) . . ?
C3 N3 Ni 103.9(5) . . ?
C5 N3 Ni 112.4(5) . . ?
C4 N4 C6 114.3(6) . 7_565 ?
C4 N4 Ni 104.7(5) . . ?
C6 N4 Ni 112.2(6) 7_565 . ?
C5 N5 C6 116.4(7) . . ?
C5 N5 C7 113.0(8) . . ?
C6 N5 C7 115.2(7) . . ?
N1 C1 Fe 177.9(8) . . ?
N2 C2 Fe 174.0(9) . . ?
N3 C3 C4 108.3(8) . . ?
N4 C4 C3 107.8(7) . . ?
N5 C5 N3 115.7(8) . . ?
N5 C6 N4 115.4(7) . 7_565 ?
N5 C7 C8 117.0(8) . . ?
O1 C8 C7 104.5(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
Ni N4 2.076(7) 7_565 ?
Ni N4 2.076(7) . ?
Ni N1 2.083(7) 7_565 ?
Ni N1 2.083(7) . ?
Ni N3 2.106(7) 7_565 ?
Ni N3 2.106(7) . ?
Fe C2 1.933(9) 3_565 ?
Fe C2 1.933(9) . ?
Fe C2 1.933(9) 2_665 ?
Fe C1 1.942(9) . ?
Fe C1 1.942(9) 3_565 ?
Fe C1 1.942(9) 2_665 ?
O1 C8 1.42(2) . ?
N1 C1 1.148(9) . ?
N2 C2 1.153(9) . ?
N3 C3 1.473(9) . ?
N3 C5 1.475(9) . ?
N4 C4 1.466(9) . ?
N4 C6 1.484(9) 7_565 ?
N5 C5 1.415(9) . ?
N5 C6 1.444(9) . ?
N5 C7 1.465(8) . ?
C3 C4 1.538(8) . ?
C6 N4 1.484(9) 7_565 ?
C7 C8 1.488(9) . ?
OW3 OW3 1.48(4) 5 ?
