#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/32/7003259.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_7003259
loop_
_publ_author_name
'Beves, Jonathon E.'
'Dunphy, Emma L.'
'Constable, Edwin C.'
'Housecroft, Catherine E.'
'Kepert, Cameron J.'
'Neuburger, Markus'
'Price, David J.'
'Schaffner, Silvia'
_publ_section_title
;
 Vectorial property dependence in
 bis{4′-(n-pyridyl)-2,2′:6′,2″-terpyridine}iron(ii)
 and ruthenium(ii) complexes with n = 2, 3 and 4
;
_journal_issue                   3
_journal_name_full               'Dalton Transactions'
_journal_page_first              386
_journal_paper_doi               10.1039/b714970k
_journal_year                    2008
_chemical_formula_moiety         'C40 H28 Fe N8, 2(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C44 H34 F12 Fe N10 P2'
_chemical_formula_weight         1048.59
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             07-07-16
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7704(2)
_cell_length_b                   8.7704(2)
_cell_length_c                   56.5252(14)
_cell_measurement_reflns_used    5511
_cell_measurement_temperature    173
_cell_measurement_theta_max      30
_cell_measurement_theta_min      1
_cell_volume                     4347.91(18)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.086
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       79
_diffrn_reflns_limit_l_min       -79
_diffrn_reflns_number            34009
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         3.363
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.520
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_description       block
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.51
_refine_diff_density_min         -1.04
_refine_ls_extinction_coef       1288.554
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9421
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         2431
_refine_ls_number_restraints     335
_refine_ls_R_factor_all          0.1160
_refine_ls_R_factor_gt           0.0998
_refine_ls_shift/su_max          0.000717
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)]
where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)²]²
Ai are:
9.75 -2.63 4.11 5.05 -1.29
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0590
_refine_ls_wR_factor_gt          0.0578
_refine_ls_wR_factor_ref         0.0578
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              79
_reflns_limit_l_min              0
_reflns_number_gt                2431
_reflns_number_total             3188
_reflns_threshold_expression     I>3.0σ(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.959(3)
_oxford_structure_analysis_title '3271628 jb421_173k'
_cod_data_source_file            b714970k.txt
_cod_data_source_block           jb421_173k
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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      'I 41/a'
_cod_original_formula_sum        'C44 H34 F12 Fe1 N10 P2'
_cod_database_code               7003259
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z+1/2
-x+1/2,-y+1/2,-z+1/2
-y+3/4,x+1/4,z+1/4
y+3/4,-x+1/4,-z+1/4
-y+5/4,x+3/4,z+3/4
y+5/4,-x+3/4,-z+3/4
-x+1/2,-y,z+1/2
x+1/2,y,-z+1/2
-x+1,-y+1/2,z+1
x+1,y+1/2,-z+1
y+3/4,-x+3/4,z+3/4
-y+3/4,x+3/4,-z+3/4
y+5/4,-x+5/4,z+5/4
-y+5/4,x+5/4,-z+5/4
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Fe1 Fe 0.0000 0.2500 0.6250 0.0175 1.0000 Uani S T . . . .
N1 N -0.08246(18) 0.04271(18) 0.61931(3) 0.0206 1.0000 Uani . . . . . .
N2 N 0.0000 0.2500 0.59170(4) 0.0208 1.0000 Uani S T . . . .
N3 N 0.0000 0.2500 0.46690(5) 0.0486 1.0000 Uani S T . . . .
C1 C -0.1240(2) -0.0610(2) 0.63557(4) 0.0260 1.0000 Uani . . . . . .
C2 C -0.1898(3) -0.2000(2) 0.62945(4) 0.0333 1.0000 Uani . . . . . .
C3 C -0.2116(3) -0.2343(3) 0.60580(5) 0.0370 1.0000 Uani . . . . . .
C4 C -0.1664(3) -0.1300(3) 0.58879(4) 0.0318 1.0000 Uani . . . . . .
C5 C -0.1021(2) 0.0069(2) 0.59603(3) 0.0230 1.0000 Uani . . . . . .
C6 C -0.0518(2) 0.1270(2) 0.57981(3) 0.0229 1.0000 Uani . . . . . .
C7 C -0.0535(2) 0.1239(2) 0.55525(3) 0.0282 1.0000 Uani . . . . . .
C8 C 0.0000 0.2500 0.54272(4) 0.0284 1.0000 Uani S T . . . .
C9 C 0.0000 0.2500 0.51656(5) 0.0317 1.0000 Uani S T . . . .
C10 C -0.1121(3) 0.1740(4) 0.50386(4) 0.0440 1.0000 Uani . . . . . .
C11 C -0.1053(4) 0.1782(4) 0.47913(4) 0.0507 1.0000 Uani . . . . . .
P1 P 0.52525(17) 0.4033(2) 0.54723(2) 0.0445 0.5000 Uani D U . . . .
F1 F 0.4391(5) 0.2747(5) 0.53220(7) 0.0680 0.5000 Uani D U . . . .
F2 F 0.6150(7) 0.5305(7) 0.56193(9) 0.0780 0.5000 Uani D U . . . .
F3 F 0.6378(6) 0.4315(8) 0.52575(7) 0.1087 0.5000 Uani D U . . . .
F4 F 0.4161(5) 0.3753(6) 0.56921(7) 0.0740 0.5000 Uani D U . . . .
F5 F 0.4098(6) 0.5272(5) 0.53706(9) 0.0775 0.5000 Uani D U . . . .
F6 F 0.6364(6) 0.2762(6) 0.55767(9) 0.0918 0.5000 Uani D U . . . .
N4 N 0.400(2) -0.0722(17) 0.56806(17) 0.1122 0.5000 Uani D U . . . .
C12 C 0.4624(11) -0.0843(12) 0.55001(12) 0.0771 0.5000 Uani D U . . . .
C13 C 0.5319(11) -0.0947(15) 0.52633(14) 0.0810 0.5000 Uani D U . . . .
H11 H -0.1075 -0.0382 0.6522 0.0315 1.0000 Uiso R . . . . .
H21 H -0.2199 -0.2720 0.6416 0.0403 1.0000 Uiso R . . . . .
H31 H -0.2579 -0.3302 0.6012 0.0448 1.0000 Uiso R . . . . .
H41 H -0.1795 -0.1522 0.5721 0.0385 1.0000 Uiso R . . . . .
H71 H -0.0915 0.0350 0.5469 0.0342 1.0000 Uiso R . . . . .
H101 H -0.1930 0.1195 0.5119 0.0532 1.0000 Uiso R . . . . .
H111 H -0.1838 0.1242 0.4704 0.0611 1.0000 Uiso R . . . . .
H131 H 0.6326 -0.1398 0.5276 0.0973 0.5000 Uiso R . . . . .
H132 H 0.5404 0.0067 0.5196 0.0973 0.5000 Uiso R . . . . .
H133 H 0.4686 -0.1576 0.5162 0.0973 0.5000 Uiso R . . . . .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805
1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 11_454 Fe1 . N1 16_445 91.508(14) yes
N1 11_454 Fe1 . N1 6_456 91.508(14) yes
N1 16_445 Fe1 . N1 6_456 161.33(9) yes
N1 11_454 Fe1 . N2 6_456 99.34(4) yes
N1 16_445 Fe1 . N2 6_456 80.66(4) yes
N1 6_456 Fe1 . N2 6_456 80.66(4) yes
N1 11_454 Fe1 . N1 . 161.33(9) yes
N1 16_445 Fe1 . N1 . 91.508(14) yes
N1 6_456 Fe1 . N1 . 91.508(14) yes
N2 6_456 Fe1 . N1 . 99.34(4) yes
N1 11_454 Fe1 . N2 . 80.66(4) yes
N1 16_445 Fe1 . N2 . 99.34(4) yes
N1 6_456 Fe1 . N2 . 99.34(4) yes
N2 6_456 Fe1 . N2 . 179.994 yes
N1 . Fe1 . N2 . 80.66(4) yes
Fe1 . N1 . C1 . 127.50(13) yes
Fe1 . N1 . C5 . 114.45(12) yes
C1 . N1 . C5 . 118.02(17) yes
C6 11_454 N2 . Fe1 . 119.86(11) yes
C6 11_454 N2 . C6 . 120.3(2) yes
Fe1 . N2 . C6 . 119.86(11) yes
C11 11_454 N3 . C11 . 116.5(3) yes
N1 . C1 . C2 . 122.37(19) yes
N1 . C1 . H11 . 118.8 no
C2 . C1 . H11 . 118.8 no
C1 . C2 . C3 . 119.15(19) yes
C1 . C2 . H21 . 120.4 no
C3 . C2 . H21 . 120.4 no
C2 . C3 . C4 . 119.2(2) yes
C2 . C3 . H31 . 120.4 no
C4 . C3 . H31 . 120.4 no
C3 . C4 . C5 . 118.9(2) yes
C3 . C4 . H41 . 120.6 no
C5 . C4 . H41 . 120.6 no
C4 . C5 . N1 . 122.35(17) yes
C4 . C5 . C6 . 124.07(18) yes
N1 . C5 . C6 . 113.58(16) yes
C5 . C6 . N2 . 111.39(16) yes
C5 . C6 . C7 . 127.45(17) yes
N2 . C6 . C7 . 121.15(18) yes
C6 . C7 . C8 . 119.23(19) yes
C6 . C7 . H71 . 120.4 no
C8 . C7 . H71 . 120.4 no
C7 . C8 . C7 11_454 119.0(2) yes
C7 . C8 . C9 . 120.52(12) yes
C7 11_454 C8 . C9 . 120.52(12) yes
C8 . C9 . C10 11_454 121.16(15) yes
C8 . C9 . C10 . 121.16(15) yes
C10 11_454 C9 . C10 . 117.7(3) yes
C9 . C10 . C11 . 118.3(3) yes
C9 . C10 . H101 . 120.8 no
C11 . C10 . H101 . 120.9 no
C10 . C11 . N3 . 124.6(3) yes
C10 . C11 . H111 . 117.7 no
N3 . C11 . H111 . 117.7 no
F1 . P1 . F2 . 178.6(3) yes
F1 . P1 . F3 . 89.8(2) yes
F2 . P1 . F3 . 89.0(3) yes
F1 . P1 . F4 . 91.2(2) yes
F2 . P1 . F4 . 89.9(3) yes
F3 . P1 . F4 . 178.5(3) yes
F1 . P1 . F5 . 89.4(2) yes
F2 . P1 . F5 . 91.4(3) yes
F3 . P1 . F5 . 90.7(3) yes
F4 . P1 . F5 . 90.3(3) yes
F1 . P1 . F6 . 89.6(2) yes
F2 . P1 . F6 . 89.7(3) yes
F3 . P1 . F6 . 90.7(3) yes
F4 . P1 . F6 . 88.3(3) yes
F5 . P1 . F6 . 178.2(3) yes
N4 . C12 . C13 . 175.8(13) yes
C12 . C13 . H131 . 109.5 no
C12 . C13 . H132 . 109.4 no
C12 . C13 . H133 . 109.5 no
H131 . C13 . H132 . 109.5 no
H131 . C13 . H133 . 109.5 no
H132 . C13 . H133 . 109.5 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 . N1 11_454 1.9828(16) yes
Fe1 . N1 16_445 1.9828(16) yes
Fe1 . N1 6_456 1.9828(16) yes
Fe1 . N2 6_456 1.882(2) yes
Fe1 . N1 . 1.9828(16) yes
Fe1 . N2 . 1.882(2) yes
N1 . C1 . 1.343(2) yes
N1 . C5 . 1.364(2) yes
N2 . C6 11_454 1.349(2) yes
N2 . C6 . 1.349(2) yes
N3 . C11 11_454 1.314(4) yes
N3 . C11 . 1.314(4) yes
C1 . C2 . 1.393(3) yes
C1 . H11 . 0.970 no
C2 . C3 . 1.383(3) yes
C2 . H21 . 0.970 no
C3 . C4 . 1.385(3) yes
C3 . H31 . 0.970 no
C4 . C5 . 1.388(3) yes
C4 . H41 . 0.970 no
C5 . C6 . 1.465(3) yes
C6 . C7 . 1.389(3) yes
C7 . C8 . 1.395(2) yes
C7 . H71 . 0.970 no
C8 . C9 . 1.478(3) yes
C9 . C10 11_454 1.388(3) yes
C9 . C10 . 1.388(3) yes
C10 . C11 . 1.400(3) yes
C10 . H101 . 0.970 no
C11 . H111 . 0.970 no
P1 . F1 . 1.602(3) yes
P1 . F2 . 1.598(4) yes
P1 . F3 . 1.584(4) yes
P1 . F4 . 1.588(4) yes
P1 . F5 . 1.593(4) yes
P1 . F6 . 1.594(4) yes
N4 . C12 . 1.165(13) yes
C12 . C13 . 1.474(10) yes
C13 . H131 . 0.970 no
C13 . H132 . 0.970 no
C13 . H133 . 0.970 no
