#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:21:14 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179786 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/82/7008242.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_7008242
loop_
_publ_author_name
'Toma, Liviu'
'Toma, Luminita Marilena'
'Lescouëzec, Rodrigue'
'Armentano, Donatella'
'De Munno, Giovanni'
'Andruh, Marius'
'Cano, Joan'
'Lloret, Francesc'
'Julve, Miguel'
_publ_section_title
;
 Synthesis, crystal structures and magnetic properties of cyanide- and
 phenolate-bridged [M(III)NiII]2 tetranuclear complexes (M=Fe and Cr).
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1357
_journal_page_last               1364
_journal_paper_doi               10.1039/b500168b
_journal_year                    2005
_chemical_formula_sum            'C30 H26 Fe N9 Ni O2'
_chemical_formula_weight         659.16
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.95(3)
_cell_angle_beta                 103.44(3)
_cell_angle_gamma                109.17(3)
_cell_formula_units_Z            2
_cell_length_a                   9.841(2)
_cell_length_b                   11.514(2)
_cell_length_c                   14.595(3)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      15
_cell_volume                     1454.1(7)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'R3m/V automatic four-circle diffractometer'
_diffrn_measurement_method       omega/2-theta-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  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6124
_diffrn_reflns_theta_full        26.05
_diffrn_reflns_theta_max         26.05
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        2.9
_exptl_absorpt_coefficient_mu    1.192
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             678
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         5739
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0417
_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)+(0.0743P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1099
_reflns_number_gt                4246
_reflns_number_total             5739
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b500168b.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_cell_volume        1454.0(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7008242
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Fe1 Fe -0.14858(5) 0.21134(4) 0.30039(3) 0.03232(13) Uani 1 1 d . . .
N1 N 0.0562(3) 0.2960(3) 0.40300(18) 0.0370(6) Uani 1 1 d . . .
N2 N -0.1180(3) 0.0519(3) 0.31797(19) 0.0399(6) Uani 1 1 d . . .
C1 C 0.1410(4) 0.4205(3) 0.4469(2) 0.0444(8) Uani 1 1 d . . .
H1A H 0.1008 0.4804 0.4335 0.053 Uiso 1 1 calc R . .
C2 C 0.2863(4) 0.4638(4) 0.5113(3) 0.0599(10) Uani 1 1 d . . .
H2A H 0.3417 0.5515 0.5406 0.072 Uiso 1 1 calc R . .
C3 C 0.3484(4) 0.3794(5) 0.5321(3) 0.0631(11) Uani 1 1 d . . .
H3A H 0.4470 0.4089 0.5746 0.076 Uiso 1 1 calc R . .
C4 C 0.2635(4) 0.2468(4) 0.4893(2) 0.0507(9) Uani 1 1 d . . .
C5 C 0.3152(5) 0.1491(5) 0.5074(3) 0.0658(12) Uani 1 1 d . . .
H5A H 0.4135 0.1723 0.5483 0.079 Uiso 1 1 calc R . .
C6 C 0.2246(5) 0.0233(5) 0.4664(3) 0.0662(13) Uani 1 1 d . . .
H6A H 0.2612 -0.0383 0.4806 0.079 Uiso 1 1 calc R . .
C7 C 0.0730(5) -0.0171(4) 0.4014(3) 0.0512(9) Uani 1 1 d . . .
C8 C -0.0285(6) -0.1450(4) 0.3559(3) 0.0624(11) Uani 1 1 d . . .
H8A H -0.0009 -0.2119 0.3679 0.075 Uiso 1 1 calc R . .
C9 C -0.1681(5) -0.1701(4) 0.2937(3) 0.0645(12) Uani 1 1 d . . .
H9A H -0.2358 -0.2549 0.2630 0.077 Uiso 1 1 calc R . .
C10 C -0.2110(4) -0.0705(3) 0.2755(3) 0.0512(9) Uani 1 1 d . . .
H10A H -0.3069 -0.0902 0.2326 0.061 Uiso 1 1 calc R . .
C11 C 0.0219(4) 0.0788(3) 0.3805(2) 0.0390(7) Uani 1 1 d . . .
C12 C 0.1168(4) 0.2100(3) 0.4257(2) 0.0395(7) Uani 1 1 d . . .
N8 N 0.2391(3) 0.2873(2) 0.04106(19) 0.0396(6) Uani 1 1 d . . .
C13 C -0.2535(4) 0.2134(3) 0.3984(2) 0.0410(7) Uani 1 1 d . . .
N3 N -0.3180(4) 0.2157(3) 0.4536(2) 0.0616(9) Uani 1 1 d . . .
C14 C -0.1661(4) 0.3690(3) 0.2861(2) 0.0409(7) Uani 1 1 d . . .
N4 N -0.1737(4) 0.4641(3) 0.2787(3) 0.0661(9) Uani 1 1 d . . .
C15 C -0.3394(4) 0.1205(3) 0.1990(2) 0.0398(7) Uani 1 1 d . . .
N5 N -0.4518(3) 0.0627(3) 0.1354(2) 0.0557(8) Uani 1 1 d . . .
C16 C -0.0499(3) 0.2059(3) 0.1984(2) 0.0336(7) Uani 1 1 d . . .
N6 N 0.0063(3) 0.1923(3) 0.13935(19) 0.0374(6) Uani 1 1 d . . .
Ni1 Ni 0.13849(4) 0.12199(3) 0.06799(3) 0.02798(12) Uani 1 1 d . . .
N7 N 0.2892(3) 0.1543(2) 0.20035(18) 0.0345(6) Uani 1 1 d . . .
C17 C 0.2995(3) 0.0636(3) 0.2357(2) 0.0365(7) Uani 1 1 d . . .
H17A H 0.3805 0.0873 0.2927 0.044 Uiso 1 1 calc R . .
C18 C 0.2015(3) -0.0722(3) 0.1990(2) 0.0350(7) Uani 1 1 d . . .
C19 C 0.2481(4) -0.1528(3) 0.2487(2) 0.0432(8) Uani 1 1 d . . .
H19A H 0.3405 -0.1166 0.2991 0.052 Uiso 1 1 calc R . .
C20 C 0.1644(4) -0.2822(3) 0.2270(3) 0.0464(8) Uani 1 1 d . . .
C21 C 0.0249(4) -0.3329(3) 0.1547(3) 0.0457(8) Uani 1 1 d . . .
H21A H -0.0365 -0.4190 0.1415 0.055 Uiso 1 1 calc R . .
C22 C -0.0279(4) -0.2593(3) 0.1004(2) 0.0362(7) Uani 1 1 d . . .
C23 C 0.0619(3) -0.1270(3) 0.1198(2) 0.0310(6) Uani 1 1 d . . .
C24 C 0.2212(5) -0.3647(4) 0.2824(3) 0.0662(12) Uani 1 1 d . . .
H24A H 0.3197 -0.3130 0.3295 0.099 Uiso 1 1 calc R . .
H24B H 0.2278 -0.4331 0.2368 0.099 Uiso 1 1 calc R . .
H24C H 0.1520 -0.4003 0.3161 0.099 Uiso 1 1 calc R . .
O1 O 0.0164(2) -0.05686(18) 0.06890(14) 0.0316(4) Uani 1 1 d . . .
O2 O 0.2803(3) 0.0509(2) 0.00323(17) 0.0466(6) Uani 1 1 d D . .
H1W H 0.374(2) 0.049(3) 0.037(2) 0.060 Uiso 1 1 d D . .
H2W H 0.241(4) -0.019(2) -0.0543(16) 0.060 Uiso 1 1 d D . .
C25 C 0.4092(4) 0.2836(3) 0.2560(2) 0.0473(9) Uani 1 1 d . . .
H25A H 0.4019 0.3063 0.3216 0.057 Uiso 1 1 calc R . .
H25B H 0.5073 0.2784 0.2628 0.057 Uiso 1 1 calc R . .
C26 C 0.4037(5) 0.3874(4) 0.2119(3) 0.0661(12) Uani 1 1 d . . .
H26A H 0.4928 0.4642 0.2507 0.079 Uiso 1 1 calc R . .
H26B H 0.3160 0.4046 0.2190 0.079 Uiso 1 1 calc R . .
C27 C 0.3963(4) 0.3687(4) 0.1076(3) 0.0643(12) Uani 1 1 d . . .
H27A H 0.4645 0.3280 0.0942 0.077 Uiso 1 1 calc R . .
H27B H 0.4291 0.4515 0.0950 0.077 Uiso 1 1 calc R . .
C28 C 0.1786(4) 0.3262(3) -0.0272(3) 0.0451(8) Uani 1 1 d . . .
H28A H 0.2368 0.4060 -0.0310 0.054 Uiso 1 1 calc R . .
C29 C 0.2922(7) 0.7322(6) 0.0014(4) 0.0788(14) Uani 1 1 d . . .
H29A H 0.345(5) 0.793(4) -0.019(3) 0.060 Uiso 1 1 d . . .
H29B H 0.197(5) 0.698(4) 0.008(3) 0.060 Uiso 1 1 d . . .
H29C H 0.268(4) 0.662(4) -0.060(3) 0.060 Uiso 1 1 d . . .
C30 C 0.3995(6) 0.7074(4) 0.0713(4) 0.0726(13) Uani 1 1 d . . .
N9 N 0.4834(6) 0.6892(5) 0.1270(5) 0.119(2) Uani 1 1 d . . .
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
C15 Fe1 C14 88.24(14) . . ?
C15 Fe1 C13 89.72(14) . . ?
C14 Fe1 C13 89.15(14) . . ?
C15 Fe1 C16 88.32(13) . . ?
C14 Fe1 C16 90.83(13) . . ?
C13 Fe1 C16 178.04(13) . . ?
C15 Fe1 N1 175.72(12) . . ?
C14 Fe1 N1 95.33(13) . . ?
C13 Fe1 N1 92.69(12) . . ?
C16 Fe1 N1 89.27(11) . . ?
C15 Fe1 N2 94.54(13) . . ?
C14 Fe1 N2 176.89(13) . . ?
C13 Fe1 N2 92.25(12) . . ?
C16 Fe1 N2 87.87(12) . . ?
N1 Fe1 N2 81.84(11) . . ?
C1 N1 C12 117.5(3) . . ?
C1 N1 Fe1 129.7(2) . . ?
C12 N1 Fe1 112.7(2) . . ?
C10 N2 C11 118.3(3) . . ?
C10 N2 Fe1 129.3(3) . . ?
C11 N2 Fe1 112.3(2) . . ?
N1 C1 C2 122.4(4) . . ?
C3 C2 C1 120.3(4) . . ?
C2 C3 C4 119.8(3) . . ?
C12 C4 C3 116.7(3) . . ?
C12 C4 C5 118.4(4) . . ?
C3 C4 C5 124.9(4) . . ?
C6 C5 C4 121.4(4) . . ?
C5 C6 C7 121.3(4) . . ?
C8 C7 C11 117.0(4) . . ?
C8 C7 C6 125.1(4) . . ?
C11 C7 C6 117.9(4) . . ?
C9 C8 C7 119.2(4) . . ?
C8 C9 C10 120.9(4) . . ?
N2 C10 C9 121.5(4) . . ?
N2 C11 C7 123.1(3) . . ?
N2 C11 C12 116.8(3) . . ?
C7 C11 C12 120.1(3) . . ?
N1 C12 C4 123.2(3) . . ?
N1 C12 C11 116.0(3) . . ?
C4 C12 C11 120.8(3) . . ?
C28 N8 C27 119.2(3) . . ?
C28 N8 Ni1 124.9(2) . . ?
C27 N8 Ni1 115.9(2) . . ?
N3 C13 Fe1 177.8(3) . . ?
N4 C14 Fe1 178.7(4) . . ?
N5 C15 Fe1 177.0(3) . . ?
N6 C16 Fe1 174.0(3) . . ?
C16 N6 Ni1 155.8(2) . . ?
N8 Ni1 O1 169.65(9) . . ?
N8 Ni1 N7 98.70(11) . . ?
O1 Ni1 N7 91.15(10) . . ?
N8 Ni1 O1 89.55(10) . 2 ?
O1 Ni1 O1 80.34(9) . 2 ?
N7 Ni1 O1 169.89(9) . 2 ?
N8 Ni1 N6 93.84(11) . . ?
O1 Ni1 N6 89.33(10) . . ?
N7 Ni1 N6 89.97(10) . . ?
O1 Ni1 N6 95.34(9) 2 . ?
N8 Ni1 O2 87.13(11) . . ?
O1 Ni1 O2 90.24(9) . . ?
N7 Ni1 O2 86.89(10) . . ?
O1 Ni1 O2 87.69(9) 2 . ?
N6 Ni1 O2 176.82(9) . . ?
C17 N7 C25 115.2(3) . . ?
C17 N7 Ni1 122.4(2) . . ?
C25 N7 Ni1 121.9(2) . . ?
N7 C17 C18 128.7(3) . . ?
C19 C18 C23 118.8(3) . . ?
C19 C18 C17 116.2(3) . . ?
C23 C18 C17 125.0(3) . . ?
C20 C19 C18 123.6(3) . . ?
C19 C20 C21 117.1(3) . . ?
C19 C20 C24 121.3(3) . . ?
C21 C20 C24 121.5(3) . . ?
C20 C21 C22 122.5(3) . . ?
C21 C22 C23 120.2(3) . . ?
C21 C22 C28 116.0(3) . 2 ?
C23 C22 C28 123.8(3) . 2 ?
O1 C23 C22 121.3(3) . . ?
O1 C23 C18 121.1(3) . . ?
C22 C23 C18 117.5(3) . . ?
C23 O1 Ni1 127.73(18) . . ?
C23 O1 Ni1 126.45(18) . 2 ?
Ni1 O1 Ni1 99.66(9) . 2 ?
C26 C25 N7 115.5(3) . . ?
C25 C26 C27 118.6(4) . . ?
C26 C27 N8 110.9(3) . . ?
N8 C28 C22 127.2(3) . 2 ?
N9 C30 C29 179.1(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
Fe1 C15 1.908(3) . ?
Fe1 C14 1.924(4) . ?
Fe1 C13 1.950(3) . ?
Fe1 C16 1.959(3) . ?
Fe1 N1 2.001(3) . ?
Fe1 N2 2.008(3) . ?
N1 C1 1.334(4) . ?
N1 C12 1.366(4) . ?
N2 C10 1.329(4) . ?
N2 C11 1.361(4) . ?
C1 C2 1.381(5) . ?
C2 C3 1.352(6) . ?
C3 C4 1.406(6) . ?
C4 C12 1.397(5) . ?
C4 C5 1.420(6) . ?
C5 C6 1.351(6) . ?
C6 C7 1.436(6) . ?
C7 C8 1.400(6) . ?
C7 C11 1.409(5) . ?
C8 C9 1.362(6) . ?
C9 C10 1.395(5) . ?
C11 C12 1.413(5) . ?
N8 C28 1.272(4) . ?
N8 C27 1.490(4) . ?
N8 Ni1 1.996(3) . ?
C13 N3 1.137(4) . ?
C14 N4 1.146(4) . ?
C15 N5 1.154(4) . ?
C16 N6 1.141(4) . ?
N6 Ni1 2.105(3) . ?
Ni1 O1 2.019(2) . ?
Ni1 N7 2.025(3) . ?
Ni1 O1 2.035(2) 2 ?
Ni1 O2 2.141(2) . ?
N7 C17 1.271(4) . ?
N7 C25 1.487(4) . ?
C17 C18 1.453(4) . ?
C18 C19 1.407(4) . ?
C18 C23 1.427(4) . ?
C19 C20 1.376(5) . ?
C20 C21 1.381(5) . ?
C20 C24 1.516(5) . ?
C21 C22 1.403(4) . ?
C22 C23 1.420(4) . ?
C22 C28 1.461(4) 2 ?
C23 O1 1.310(3) . ?
O1 Ni1 2.035(2) 2 ?
C25 C26 1.472(5) . ?
C26 C27 1.477(6) . ?
C28 C22 1.461(4) 2 ?
C29 C30 1.430(8) . ?
C30 N9 1.120(6) . ?
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
O2 H2W N6 0.945(10) 2.43(3) 3.162(4) 134(3) 2
O2 H1W N5 0.945(10) 1.905(13) 2.826(4) 164(3) 1_655
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
Fe1 C16 N6 Ni1 -32(3) . . . . ?
