#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:56:49 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180364 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/33/7203352.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_7203352
loop_
_publ_author_name
'Manuel Quesada'
'Maria Monrabal'
'Guillem Aromí'
'Víctor A. de la Peña-O'Shea'
'Martí Gich'
'Elies Molins'
'Olivier Roubeau'
'Simon J. Teat'
'Elizabeth J. MacLean'
'Patrick Gamez'
'Jan Reedijk'
_publ_section_title
;
 Spin transition in a triazine-based Fe(<small>II</small>) complex:
 variable-temperature structural, thermal, magnetic and spectroscopic
 studies
;
_journal_issue                   26
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              2669
_journal_paper_doi               10.1039/b602903e
_journal_volume                  16
_journal_year                    2006
_chemical_formula_sum            'C68 H52 Fe N26 O2 S2'
_chemical_formula_weight         1385.33
_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                95.9420(10)
_cell_angle_beta                 111.8980(10)
_cell_angle_gamma                115.8500(10)
_cell_formula_units_Z            1
_cell_length_a                   11.6660(7)
_cell_length_b                   12.8283(7)
_cell_length_c                   13.4211(8)
_cell_measurement_reflns_used    4944
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      29.492
_cell_measurement_theta_min      3.122
_cell_volume                     1589.67(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      250(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.69230
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18217
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.62
_diffrn_reflns_theta_min         1.68
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.374
_exptl_absorpt_correction_T_max  0.9843
_exptl_absorpt_correction_T_min  0.9761
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         9385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0477
_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)+(0.0842P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.1412
_reflns_number_gt                7126
_reflns_number_total             9385
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b602903e.txt
_cod_data_source_block           eu_22_01b
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7203352
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
N1 N 0.27782(13) 0.07922(11) 0.27681(11) 0.0266(3) Uani 1 1 d . . .
C1 C 0.23840(15) 0.15863(12) 0.24477(12) 0.0222(3) Uani 1 1 d . . .
N2 N 0.10401(13) 0.13755(11) 0.19313(11) 0.0253(2) Uani 1 1 d . . .
C2 C 0.00312(15) 0.02112(13) 0.16928(12) 0.0247(3) Uani 1 1 d . . .
N3 N 0.02610(13) -0.07046(11) 0.18818(11) 0.0275(3) Uani 1 1 d . . .
C3 C 0.16617(16) -0.03379(13) 0.24524(13) 0.0251(3) Uani 1 1 d . . .
N4 N 0.34901(13) 0.27691(10) 0.27233(11) 0.0243(2) Uani 1 1 d . . .
C4 C 0.31753(15) 0.36706(13) 0.23748(13) 0.0247(3) Uani 1 1 d . . .
C5 C 0.23909(17) 0.34768(15) 0.12288(14) 0.0310(3) Uani 1 1 d . . .
H5 H 0.2053 0.2756 0.0676 0.037 Uiso 1 1 calc R . .
C6 C 0.2123(2) 0.43810(18) 0.09290(16) 0.0399(4) Uani 1 1 d . . .
H6 H 0.1574 0.4270 0.0165 0.048 Uiso 1 1 calc R . .
C7 C 0.2666(2) 0.54412(18) 0.17559(18) 0.0432(4) Uani 1 1 d . . .
H7 H 0.2499 0.6064 0.1566 0.052 Uiso 1 1 calc R . .
N5 N 0.37018(15) 0.46899(11) 0.31894(12) 0.0303(3) Uani 1 1 d . . .
C8 C 0.3456(2) 0.55693(16) 0.28626(17) 0.0399(4) Uani 1 1 d . . .
H8 H 0.3846 0.6303 0.3423 0.048 Uiso 1 1 calc R . .
C9 C 0.49654(15) 0.30829(13) 0.33127(13) 0.0247(3) Uani 1 1 d . . .
C10 C 0.54689(18) 0.24848(16) 0.28313(15) 0.0343(3) Uani 1 1 d . . .
H10 H 0.4860 0.1881 0.2116 0.041 Uiso 1 1 calc R . .
C11 C 0.68931(19) 0.28002(17) 0.34317(17) 0.0410(4) Uani 1 1 d . . .
H11 H 0.7258 0.2390 0.3143 0.049 Uiso 1 1 calc R . .
C12 C 0.77701(18) 0.37274(18) 0.44621(17) 0.0411(4) Uani 1 1 d . . .
H12 H 0.8741 0.3960 0.4882 0.049 Uiso 1 1 calc R . .
C13 C 0.71985(18) 0.43033(17) 0.48614(15) 0.0380(4) Uani 1 1 d . . .
H13A H 0.7807 0.4949 0.5550 0.046 Uiso 1 1 calc R . .
N6 N 0.57973(14) 0.39817(12) 0.43070(11) 0.0294(3) Uani 1 1 d . . .
N7 N -0.13941(13) -0.00934(12) 0.11901(12) 0.0290(3) Uani 1 1 d . . .
C14 C -0.18531(16) 0.07274(14) 0.08184(13) 0.0272(3) Uani 1 1 d . . .
C15 C -0.12558(18) 0.14917(16) 0.02669(14) 0.0334(3) Uani 1 1 d . . .
H15 H -0.0537 0.1481 0.0113 0.040 Uiso 1 1 calc R . .
C16 C -0.1754(2) 0.22691(18) -0.00481(16) 0.0410(4) Uani 1 1 d . . .
H16 H -0.1356 0.2817 -0.0402 0.049 Uiso 1 1 calc R . .
C17 C -0.2841(2) 0.22312(18) 0.01635(17) 0.0421(4) Uani 1 1 d . . .
H17 H -0.3189 0.2755 -0.0036 0.051 Uiso 1 1 calc R . .
C18 C -0.33999(19) 0.14099(17) 0.06721(16) 0.0388(4) Uani 1 1 d . . .
H18 H -0.4166 0.1365 0.0786 0.047 Uiso 1 1 calc R . .
N8 N -0.29158(15) 0.06624(13) 0.10185(13) 0.0349(3) Uani 1 1 d . . .
C19 C -0.24863(16) -0.12672(14) 0.10952(14) 0.0292(3) Uani 1 1 d . . .
C20 C -0.2477(2) -0.15807(18) 0.20554(17) 0.0403(4) Uani 1 1 d . . .
H20 H -0.1764 -0.1033 0.2785 0.048 Uiso 1 1 calc R . .
C21 C -0.3550(2) -0.27250(19) 0.1904(2) 0.0501(5) Uani 1 1 d . . .
H21 H -0.3584 -0.2973 0.2532 0.060 Uiso 1 1 calc R . .
C22 C -0.4566(2) -0.34949(17) 0.0824(2) 0.0516(5) Uani 1 1 d . . .
H22 H -0.5291 -0.4285 0.0701 0.062 Uiso 1 1 calc R . .
C23 C -0.4505(2) -0.30946(17) -0.00715(19) 0.0465(5) Uani 1 1 d . . .
H23 H -0.5221 -0.3623 -0.0807 0.056 Uiso 1 1 calc R . .
N9 N -0.34760(15) -0.19836(13) 0.00423(13) 0.0369(3) Uani 1 1 d . . .
N10 N 0.19792(14) -0.12210(11) 0.27335(12) 0.0304(3) Uani 1 1 d . C .
C24 C 0.34019(17) -0.10323(13) 0.31313(14) 0.0290(3) Uani 1 1 d . . .
C26 C 0.5528(3) -0.0404(2) 0.2985(2) 0.0572(6) Uani 1 1 d . . .
H26 H 0.6094 -0.0066 0.2627 0.069 Uiso 1 1 calc R A 1
C27 C 0.6052(2) -0.0751(2) 0.3898(2) 0.0601(7) Uani 1 1 d . C .
H27 H 0.6975 -0.0649 0.4177 0.072 Uiso 1 1 calc R . .
C28 C 0.5202(2) -0.12514(18) 0.44003(18) 0.0530(6) Uani 1 1 d . . .
H28 H 0.5556 -0.1495 0.5027 0.064 Uiso 1 1 calc R B 1
C25A C 0.4177(2) -0.05422(16) 0.25793(16) 0.0429(4) Uani 0.50 1 d P C 1
H25A H 0.3807 -0.0308 0.1950 0.052 Uiso 0.50 1 calc PR C 1
N12A N 0.38581(19) -0.14073(14) 0.40209(14) 0.0380(4) Uani 0.50 1 d P C 1
N12B N 0.4177(2) -0.05422(16) 0.25793(16) 0.0429(4) Uani 0.50 1 d P C 2
C25B C 0.38581(19) -0.14073(14) 0.40209(14) 0.0380(4) Uani 0.50 1 d P C 2
H25B H 0.3280 -0.1760 0.4366 0.046 Uiso 0.50 1 calc PR C 2
C29 C 0.08929(17) -0.23657(14) 0.26822(14) 0.0305(3) Uani 1 1 d . . .
C30 C 0.0129(2) -0.24039(18) 0.32702(18) 0.0443(4) Uani 1 1 d . C .
H30 H 0.0281 -0.1682 0.3693 0.053 Uiso 1 1 calc R . .
C31 C -0.0866(2) -0.3538(2) 0.3215(2) 0.0555(6) Uani 1 1 d . . .
H31 H -0.1418 -0.3601 0.3592 0.067 Uiso 1 1 calc R C .
C32 C -0.1041(2) -0.45733(19) 0.2603(2) 0.0531(5) Uani 1 1 d . C .
H32 H -0.1715 -0.5353 0.2553 0.064 Uiso 1 1 calc R . .
C33 C -0.0211(2) -0.44441(16) 0.20666(17) 0.0470(5) Uani 1 1 d . . .
H33 H -0.0315 -0.5153 0.1666 0.056 Uiso 1 1 calc R C .
N11 N 0.07471(17) -0.33477(12) 0.20859(13) 0.0373(3) Uani 1 1 d . C .
Fe1 Fe 0.5000 0.5000 0.5000 0.02629(9) Uani 1 2 d S . .
N13 N 0.33523(17) 0.33775(13) 0.49415(13) 0.0379(3) Uani 1 1 d . . .
C34 C 0.23172(18) 0.25183(14) 0.48110(14) 0.0313(3) Uani 1 1 d . . .
S1 S 0.08665(6) 0.13049(5) 0.46376(5) 0.04970(14) Uani 1 1 d . . .
O1W O -0.0049(3) 0.3104(2) 0.3131(3) 0.1414(13) 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'
S S 0.1246 0.1234 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C3 113.35(12) . . ?
N1 C1 N2 126.98(13) . . ?
N1 C1 N4 116.37(12) . . ?
N2 C1 N4 116.59(12) . . ?
C1 N2 C2 113.03(12) . . ?
N2 C2 N3 126.52(13) . . ?
N2 C2 N7 117.60(13) . . ?
N3 C2 N7 115.88(12) . . ?
C2 N3 C3 113.26(12) . . ?
N1 C3 N3 126.53(13) . . ?
N1 C3 N10 116.96(13) . . ?
N3 C3 N10 116.50(13) . . ?
C1 N4 C4 120.44(12) . . ?
C1 N4 C9 120.15(11) . . ?
C4 N4 C9 119.33(11) . . ?
N4 C4 C5 119.86(13) . . ?
N4 C4 N5 116.89(13) . . ?
C5 C4 N5 123.21(14) . . ?
C4 C5 C6 117.89(16) . . ?
C5 C6 C7 119.70(16) . . ?
C6 C7 C8 118.60(16) . . ?
C4 N5 C8 117.27(14) . . ?
C4 N5 Fe1 122.55(10) . . ?
C8 N5 Fe1 120.14(11) . . ?
C7 C8 N5 123.27(17) . . ?
N4 C9 C10 119.95(13) . . ?
N4 C9 N6 116.60(13) . . ?
C10 C9 N6 123.43(14) . . ?
C9 C10 C11 118.31(16) . . ?
C10 C11 C12 119.05(16) . . ?
C11 C12 C13 118.94(16) . . ?
C12 C13 N6 122.97(16) . . ?
C9 N6 C13 117.22(14) . . ?
C9 N6 Fe1 122.59(10) . . ?
C13 N6 Fe1 120.09(11) . . ?
C2 N7 C14 123.66(12) . . ?
C2 N7 C19 119.27(12) . . ?
C14 N7 C19 116.93(12) . . ?
N7 C14 C15 121.88(14) . . ?
N7 C14 N8 114.18(14) . . ?
C15 C14 N8 123.91(14) . . ?
C14 C15 C16 117.85(15) . . ?
C15 C16 C17 119.32(17) . . ?
C16 C17 C18 118.40(16) . . ?
C17 C18 N8 123.92(16) . . ?
C14 N8 C18 116.52(15) . . ?
N7 C19 C20 120.70(15) . . ?
N7 C19 N9 114.99(14) . . ?
C20 C19 N9 124.30(16) . . ?
C19 C20 C21 117.72(19) . . ?
C20 C21 C22 119.2(2) . . ?
C21 C22 C23 118.92(18) . . ?
C22 C23 N9 123.65(19) . . ?
C19 N9 C23 116.21(17) . . ?
C3 N10 C24 122.56(12) . . ?
C3 N10 C29 120.82(13) . . ?
C24 N10 C29 116.58(12) . . ?
N10 C24 C25A 119.66(15) . . ?
N10 C24 N12A 116.06(15) . . ?
C25A C24 N12A 124.23(16) . . ?
C27 C26 C25A 120.8(2) . . ?
C26 C27 C28 118.59(19) . . ?
C27 C28 N12A 122.26(19) . . ?
C24 C25A C26 117.21(18) . . ?
C24 N12A C28 116.85(18) . . ?
N10 C29 C30 120.89(15) . . ?
N10 C29 N11 114.94(14) . . ?
C30 C29 N11 124.09(15) . . ?
C29 C30 C31 117.85(18) . . ?
C30 C31 C32 119.38(19) . . ?
C31 C32 C33 118.63(18) . . ?
C32 C33 N11 123.21(18) . . ?
C29 N11 C33 116.81(16) . . ?
N5 Fe1 N5 180.0 . 2_666 ?
N5 Fe1 N6 82.71(5) . . ?
N5 Fe1 N6 97.29(5) 2_666 . ?
N5 Fe1 N6 97.29(5) . 2_666 ?
N5 Fe1 N6 82.71(5) 2_666 2_666 ?
N5 Fe1 N13 91.13(6) . . ?
N5 Fe1 N13 88.87(5) . 2_666 ?
N5 Fe1 N13 91.13(6) 2_666 2_666 ?
N5 Fe1 N13 88.87(6) 2_666 . ?
N6 Fe1 N6 180.00(7) . 2_666 ?
N6 Fe1 N13 91.20(5) . . ?
N6 Fe1 N13 88.80(5) . 2_666 ?
N6 Fe1 N13 91.20(5) 2_666 2_666 ?
N6 Fe1 N13 88.80(5) 2_666 . ?
N13 Fe1 N13 180.0 . 2_666 ?
Fe1 N13 C34 170.89(15) . . ?
N13 C34 S1 179.46(19) . . ?
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
N1 C1 1.3364(18) . ?
N1 C3 1.3387(19) . ?
C1 N2 1.3388(18) . ?
C1 N4 1.3873(18) . ?
N2 C2 1.3437(18) . ?
C2 N3 1.3424(18) . ?
C2 N7 1.3837(18) . ?
N3 C3 1.3415(19) . ?
C3 N10 1.3832(18) . ?
N4 C4 1.4301(18) . ?
N4 C9 1.4369(18) . ?
C4 C5 1.392(2) . ?
C4 N5 1.3360(19) . ?
C5 C6 1.387(2) . ?
C6 C7 1.377(3) . ?
C7 C8 1.371(3) . ?
N5 C8 1.356(2) . ?
N5 Fe1 2.2105(14) . ?
C9 C10 1.387(2) . ?
C9 N6 1.3386(19) . ?
C10 C11 1.386(2) . ?
C11 C12 1.384(3) . ?
C12 C13 1.376(3) . ?
C13 N6 1.355(2) . ?
N6 Fe1 2.2112(13) . ?
N7 C14 1.4302(19) . ?
N7 C19 1.4399(19) . ?
C14 C15 1.391(2) . ?
C14 N8 1.334(2) . ?
C15 C16 1.386(2) . ?
C16 C17 1.382(3) . ?
C17 C18 1.372(3) . ?
C18 N8 1.350(2) . ?
C19 C20 1.387(2) . ?
C19 N9 1.328(2) . ?
C20 C21 1.382(3) . ?
C21 C22 1.372(3) . ?
C22 C23 1.368(3) . ?
C23 N9 1.350(2) . ?
N10 C24 1.435(2) . ?
N10 C29 1.4346(19) . ?
C24 C25A 1.365(2) . ?
C24 N12A 1.345(2) . ?
C26 C27 1.367(4) . ?
C26 C25A 1.382(3) . ?
C27 C28 1.372(4) . ?
C28 N12A 1.367(3) . ?
C29 C30 1.384(2) . ?
C29 N11 1.326(2) . ?
C30 C31 1.382(3) . ?
C31 C32 1.376(3) . ?
C32 C33 1.374(3) . ?
C33 N11 1.352(2) . ?
Fe1 N5 2.2105(14) 2_666 ?
Fe1 N6 2.2113(13) 2_666 ?
Fe1 N13 2.0971(15) . ?
Fe1 N13 2.0971(15) 2_666 ?
N13 C34 1.160(2) . ?
C34 S1 1.6357(17) . ?
