#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:43:41 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179761 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/57/7005753.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_7005753
loop_
_publ_author_name
'Toma, Luminita Marilena'
'Lescouëzec, Rodrigue'
'Uriel, Santiago'
'Llusar, Rosa'
'Ruiz-Pérez, Catalina'
'Vaissermann, Jacqueline'
'Lloret, Francesc'
'Julve, Miguel'
_publ_section_title
;
 4,2-Ribbon like ferromagnetic cyano-bridged Fe(III)2Ni(II) chains: a
 magneto-structural study.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3690
_journal_page_last               3698
_journal_paper_doi               10.1039/b705084b
_journal_year                    2007
_chemical_formula_sum            'C32 H28 Fe2 N12 Ni O6'
_chemical_formula_weight         847.07
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 93.457(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.3716(6)
_cell_length_b                   15.6150(11)
_cell_length_c                   15.2953(6)
_cell_measurement_temperature    293(2)
_cell_volume                     1757.4(2)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mok\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0704
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12622
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         6.42
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.407
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.510
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular sheet'
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.013
_refine_diff_density_max         0.885
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.100
_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     241
_refine_ls_number_reflns         4875
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0531
_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)+(0.0346P)²+2.6650P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1142
_reflns_number_gt                3372
_reflns_number_total             4875
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b705084b.txt
_cod_data_source_block           compound3
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7005753
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, 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_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
C1 C 0.6820(4) 0.0701(2) 0.61621(19) 0.0237(7) Uani 1 1 d . . .
C2 C 0.3087(4) 0.0778(2) 0.63006(19) 0.0232(7) Uani 1 1 d . . .
C3 C 0.7438(4) 0.1196(2) 0.7815(2) 0.0245(7) Uani 1 1 d . . .
C4 C 0.5289(4) 0.2159(2) 0.6650(2) 0.0271(7) Uani 1 1 d . . .
C5 C 0.3402(4) 0.2085(2) 0.8390(2) 0.0297(7) Uani 1 1 d . . .
H5 H 0.3606 0.2561 0.8043 0.036 Uiso 1 1 calc R . .
C6 C 0.2621(5) 0.2203(3) 0.9193(2) 0.0377(9) Uani 1 1 d . . .
H6 H 0.2343 0.2750 0.9383 0.045 Uiso 1 1 calc R . .
C7 C 0.2274(5) 0.1511(3) 0.9691(2) 0.0385(9) Uani 1 1 d . . .
H7 H 0.1731 0.1585 1.0220 0.046 Uiso 1 1 calc R . .
C8 C 0.2725(4) 0.0688(3) 0.9418(2) 0.0300(8) Uani 1 1 d . . .
C9 C 0.3557(4) 0.0624(2) 0.86221(18) 0.0232(7) Uani 1 1 d . . .
C10 C 0.4154(4) -0.0178(2) 0.8321(2) 0.0242(7) Uani 1 1 d . . .
C11 C 0.3876(5) -0.0923(2) 0.8799(2) 0.0332(8) Uani 1 1 d . . .
C12 C 0.4479(6) -0.1690(3) 0.8450(3) 0.0432(10) Uani 1 1 d . . .
H12 H 0.4337 -0.2203 0.8746 0.052 Uiso 1 1 calc R . .
C13 C 0.5284(6) -0.1678(3) 0.7666(3) 0.0451(10) Uani 1 1 d . . .
H13 H 0.5669 -0.2187 0.7421 0.054 Uiso 1 1 calc R . .
C14 C 0.5527(5) -0.0910(2) 0.7237(2) 0.0353(8) Uani 1 1 d . . .
H14 H 0.6085 -0.0915 0.6708 0.042 Uiso 1 1 calc R . .
C15 C 0.2462(5) -0.0085(3) 0.9898(2) 0.0413(10) Uani 1 1 d . . .
H15 H 0.1895 -0.0060 1.0425 0.050 Uiso 1 1 calc R . .
C16 C 0.3012(5) -0.0839(3) 0.9606(2) 0.0424(10) Uani 1 1 d . . .
H16 H 0.2827 -0.1327 0.9938 0.051 Uiso 1 1 calc R . .
Fe1 Fe 0.52422(6) 0.10081(3) 0.70696(3) 0.01827(12) Uani 1 1 d . . .
N1 N 0.7865(4) 0.05112(19) 0.56718(17) 0.0278(6) Uani 1 1 d . . .
N2 N 0.1871(4) 0.0593(2) 0.58450(17) 0.0289(6) Uani 1 1 d . . .
N3 N 0.8680(4) 0.1300(2) 0.8283(2) 0.0458(9) Uani 1 1 d . . .
N4 N 0.5221(5) 0.2857(2) 0.6426(2) 0.0458(8) Uani 1 1 d . . .
N5 N 0.3863(3) 0.13126(17) 0.81076(15) 0.0210(5) Uani 1 1 d . . .
N6 N 0.4993(3) -0.01667(17) 0.75526(16) 0.0232(6) Uani 1 1 d . . .
Ni1 Ni 0.0000 0.0000 0.5000 0.01841(14) Uani 1 2 d S . .
O1W O -0.0002(3) 0.10444(16) 0.41501(15) 0.0347(6) Uani 1 1 d . . .
O2W O -0.0037(4) 0.0572(2) 0.24218(18) 0.0560(8) Uani 1 1 d . . .
O3W O 0.3080(5) 0.2125(2) 0.4435(2) 0.0610(9) 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'
Fe Fe 0.3463 0.8444 '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'
Ni Ni 0.3393 1.1124 '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'
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
N1 C1 Fe1 174.7(3) . . ?
N2 C2 Fe1 175.7(3) . . ?
N3 C3 Fe1 177.1(3) . . ?
N4 C4 Fe1 175.7(3) . . ?
N5 C5 C6 122.0(3) . . ?
C7 C6 C5 119.4(4) . . ?
C6 C7 C8 120.5(3) . . ?
C7 C8 C9 116.8(3) . . ?
C7 C8 C15 125.4(3) . . ?
C9 C8 C15 117.7(3) . . ?
N5 C9 C8 122.9(3) . . ?
N5 C9 C10 116.5(3) . . ?
C8 C9 C10 120.5(3) . . ?
N6 C10 C11 123.5(3) . . ?
N6 C10 C9 115.9(3) . . ?
C11 C10 C9 120.7(3) . . ?
C12 C11 C10 117.1(3) . . ?
C12 C11 C16 125.3(4) . . ?
C10 C11 C16 117.6(3) . . ?
C13 C12 C11 119.2(4) . . ?
C12 C13 C14 120.1(4) . . ?
N6 C14 C13 122.5(3) . . ?
C16 C15 C8 121.3(3) . . ?
C15 C16 C11 122.2(3) . . ?
C4 Fe1 C1 88.17(14) . . ?
C4 Fe1 C3 91.41(14) . . ?
C1 Fe1 C3 86.73(13) . . ?
C4 Fe1 C2 90.07(14) . . ?
C1 Fe1 C2 91.42(12) . . ?
C3 Fe1 C2 177.59(14) . . ?
C4 Fe1 N6 175.06(12) . . ?
C1 Fe1 N6 96.38(13) . . ?
C3 Fe1 N6 90.76(12) . . ?
C2 Fe1 N6 87.92(12) . . ?
C4 Fe1 N5 93.66(12) . . ?
C1 Fe1 N5 173.26(11) . . ?
C3 Fe1 N5 86.74(12) . . ?
C2 Fe1 N5 95.06(11) . . ?
N6 Fe1 N5 82.03(11) . . ?
C1 N1 Ni1 167.6(3) . 1_655 ?
C2 N2 Ni1 166.8(3) . . ?
C5 N5 C9 118.3(3) . . ?
C5 N5 Fe1 128.8(2) . . ?
C9 N5 Fe1 112.5(2) . . ?
C14 N6 C10 117.6(3) . . ?
C14 N6 Fe1 129.5(2) . . ?
C10 N6 Fe1 112.9(2) . . ?
N2 Ni1 N2 180.0 . 3_556 ?
N2 Ni1 O1W 89.14(11) . 3_556 ?
N2 Ni1 O1W 90.86(11) 3_556 3_556 ?
N2 Ni1 O1W 90.86(11) . . ?
N2 Ni1 O1W 89.14(11) 3_556 . ?
O1W Ni1 O1W 180.0 3_556 . ?
N2 Ni1 N1 89.11(11) . 3_656 ?
N2 Ni1 N1 90.89(11) 3_556 3_656 ?
O1W Ni1 N1 92.04(10) 3_556 3_656 ?
O1W Ni1 N1 87.96(10) . 3_656 ?
N2 Ni1 N1 90.89(11) . 1_455 ?
N2 Ni1 N1 89.11(11) 3_556 1_455 ?
O1W Ni1 N1 87.96(10) 3_556 1_455 ?
O1W Ni1 N1 92.04(10) . 1_455 ?
N1 Ni1 N1 180.00(12) 3_656 1_455 ?
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
C1 N1 1.146(4) . ?
C1 Fe1 1.925(3) . ?
C2 N2 1.139(4) . ?
C2 Fe1 1.952(3) . ?
C3 N3 1.139(4) . ?
C3 Fe1 1.945(3) . ?
C4 N4 1.144(4) . ?
C4 Fe1 1.909(4) . ?
C5 N5 1.332(4) . ?
C5 C6 1.399(5) . ?
C6 C7 1.355(6) . ?
C7 C8 1.397(5) . ?
C8 C9 1.400(4) . ?
C8 C15 1.432(5) . ?
C9 N5 1.359(4) . ?
C9 C10 1.413(5) . ?
C10 N6 1.361(4) . ?
C10 C11 1.396(5) . ?
C11 C12 1.394(5) . ?
C11 C16 1.429(5) . ?
C12 C13 1.370(6) . ?
C13 C14 1.383(6) . ?
C14 N6 1.326(4) . ?
C15 C16 1.331(6) . ?
Fe1 N6 1.990(3) . ?
Fe1 N5 1.994(2) . ?
N1 Ni1 2.089(3) 1_655 ?
N2 Ni1 2.053(3) . ?
Ni1 N2 2.053(3) 3_556 ?
Ni1 O1W 2.085(2) 3_556 ?
Ni1 O1W 2.085(2) . ?
Ni1 N1 2.089(3) 3_656 ?
Ni1 N1 2.089(3) 1_455 ?
