#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:56:49 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180364 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/33/7203351.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_7203351
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                95.3500(10)
_cell_angle_beta                 111.7160(10)
_cell_angle_gamma                116.3790(10)
_cell_formula_units_Z            1
_cell_length_a                   11.7151(7)
_cell_length_b                   12.8256(8)
_cell_length_c                   13.0725(8)
_cell_measurement_reflns_used    5736
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.582
_cell_measurement_theta_min      3.118
_cell_volume                     1554.48(17)
_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      200(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.970
_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  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0432
_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       -18
_diffrn_reflns_number            17729
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.59
_diffrn_reflns_theta_min         1.72
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.382
_exptl_absorpt_correction_T_max  0.9843
_exptl_absorpt_correction_T_min  0.9753
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.480
_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         0.537
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         9158
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0452
_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)+(0.0785P)²+0.1384P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1268
_refine_ls_wR_factor_ref         0.1323
_reflns_number_gt                7343
_reflns_number_total             9158
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b602903e.txt
_cod_data_source_block           eu_22_01c
_cod_original_cell_volume        1554.48(16)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7203351
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 0.27798(13) 0.08396(11) 0.27529(11) 0.0204(2) Uani 1 1 d . . .
C1 C 0.24048(15) 0.16462(12) 0.24381(12) 0.0176(3) Uani 1 1 d . . .
N2 N 0.10681(13) 0.14382(11) 0.18981(11) 0.0202(2) Uani 1 1 d . . .
C2 C 0.00489(15) 0.02695(13) 0.16322(12) 0.0196(3) Uani 1 1 d . . .
N3 N 0.02663(13) -0.06589(11) 0.18168(11) 0.0214(2) Uani 1 1 d . . .
C3 C 0.16582(15) -0.02998(13) 0.24079(13) 0.0197(3) Uani 1 1 d . . .
N4 N 0.35183(12) 0.28400(10) 0.27546(11) 0.0190(2) Uani 1 1 d . . .
C4 C 0.32429(15) 0.37723(13) 0.24466(13) 0.0204(3) Uani 1 1 d . . .
C5 C 0.24469(17) 0.36272(15) 0.12911(14) 0.0256(3) Uani 1 1 d . . .
H5 H 0.2057 0.2900 0.0699 0.031 Uiso 1 1 calc R . .
C6 C 0.22349(19) 0.45731(17) 0.10230(16) 0.0312(4) Uani 1 1 d . . .
H6 H 0.1664 0.4488 0.0246 0.037 Uiso 1 1 calc R . .
C7 C 0.2868(2) 0.56421(16) 0.19051(17) 0.0330(4) Uani 1 1 d . . .
H7 H 0.2752 0.6305 0.1741 0.040 Uiso 1 1 calc R . .
N5 N 0.38368(14) 0.47916(11) 0.33152(12) 0.0224(3) Uani 1 1 d . . .
C8 C 0.36672(19) 0.57223(15) 0.30231(16) 0.0287(3) Uani 1 1 d . . .
H8 H 0.4123 0.6465 0.3620 0.034 Uiso 1 1 calc R . .
C9 C 0.49844(15) 0.31685(13) 0.33932(13) 0.0204(3) Uani 1 1 d . . .
C10 C 0.55113(17) 0.25562(15) 0.29562(15) 0.0271(3) Uani 1 1 d . . .
H10 H 0.4909 0.1917 0.2239 0.032 Uiso 1 1 calc R . .
C11 C 0.69403(18) 0.29026(17) 0.35941(17) 0.0328(4) Uani 1 1 d . . .
H11 H 0.7323 0.2478 0.3339 0.039 Uiso 1 1 calc R . .
C12 C 0.78005(17) 0.38807(17) 0.46111(16) 0.0328(4) Uani 1 1 d . . .
H12 H 0.8783 0.4141 0.5057 0.039 Uiso 1 1 calc R . .
C13 C 0.72070(16) 0.44704(15) 0.49651(15) 0.0287(3) Uani 1 1 d . . .
H13A H 0.7812 0.5160 0.5643 0.034 Uiso 1 1 calc R . .
N6 N 0.57938(13) 0.41066(11) 0.43846(11) 0.0223(3) Uani 1 1 d . . .
N7 N -0.13681(13) -0.00354(11) 0.11200(12) 0.0225(3) Uani 1 1 d . . .
C14 C -0.18207(15) 0.08024(13) 0.07954(13) 0.0211(3) Uani 1 1 d . . .
C15 C -0.11881(16) 0.16522(15) 0.02953(13) 0.0247(3) Uani 1 1 d . . .
H15 H -0.0442 0.1688 0.0141 0.030 Uiso 1 1 calc R . .
C16 C -0.16798(18) 0.24442(16) 0.00295(15) 0.0301(3) Uani 1 1 d . . .
H16 H -0.1255 0.3051 -0.0292 0.036 Uiso 1 1 calc R . .
C17 C -0.28008(19) 0.23427(16) 0.02376(16) 0.0307(3) Uani 1 1 d . . .
H17 H -0.3144 0.2884 0.0076 0.037 Uiso 1 1 calc R . .
C18 C -0.33995(18) 0.14318(16) 0.06861(16) 0.0305(3) Uani 1 1 d . . .
H18 H -0.4194 0.1337 0.0795 0.037 Uiso 1 1 calc R . .
N8 N -0.29204(14) 0.06678(12) 0.09784(13) 0.0279(3) Uani 1 1 d . . .
C19 C -0.24592(15) -0.12233(13) 0.10250(14) 0.0227(3) Uani 1 1 d . . .
C20 C -0.24584(18) -0.15316(16) 0.20168(16) 0.0315(4) Uani 1 1 d . . .
H20 H -0.1748 -0.0972 0.2766 0.038 Uiso 1 1 calc R . .
C21 C -0.3531(2) -0.26840(18) 0.18742(19) 0.0381(4) Uani 1 1 d . . .
H21 H -0.3574 -0.2932 0.2528 0.046 Uiso 1 1 calc R . .
C22 C -0.45332(19) -0.34642(16) 0.07674(19) 0.0377(4) Uani 1 1 d . . .
H22 H -0.5265 -0.4266 0.0646 0.045 Uiso 1 1 calc R . .
C23 C -0.44552(19) -0.30610(15) -0.01591(18) 0.0352(4) Uani 1 1 d . . .
H23 H -0.5163 -0.3600 -0.0917 0.042 Uiso 1 1 calc R . .
N9 N -0.34307(14) -0.19441(12) -0.00493(13) 0.0288(3) Uani 1 1 d . . .
N10 N 0.19602(13) -0.11915(11) 0.26831(12) 0.0228(3) Uani 1 1 d . C .
C24 C 0.33770(16) -0.10002(13) 0.30738(13) 0.0218(3) Uani 1 1 d . . .
C26 C 0.5483(2) -0.03626(18) 0.2881(2) 0.0420(5) Uani 1 1 d . . .
H26 H 0.6036 -0.0029 0.2491 0.050 Uiso 1 1 calc R A 1
C27 C 0.6031(2) -0.06943(18) 0.3830(2) 0.0444(5) Uani 1 1 d . C .
H27 H 0.6962 -0.0583 0.4108 0.053 Uiso 1 1 calc R . .
C28 C 0.5199(2) -0.11910(17) 0.43711(17) 0.0403(5) Uani 1 1 d . . .
H28 H 0.5574 -0.1421 0.5029 0.048 Uiso 1 1 calc R B 1
C25A C 0.41316(18) -0.05093(14) 0.24845(15) 0.0312(3) Uani 0.50 1 d P C 1
H25A H 0.3745 -0.0279 0.1831 0.037 Uiso 0.50 1 calc PR C 1
N12A N 0.38513(18) -0.13653(13) 0.39935(13) 0.0287(3) Uani 0.50 1 d P C 1
N12B N 0.41316(18) -0.05093(14) 0.24845(15) 0.0312(3) Uani 0.50 1 d P C 2
C25B C 0.38513(18) -0.13653(13) 0.39935(13) 0.0287(3) Uani 0.50 1 d P C 2
H25B H 0.3278 -0.1726 0.4362 0.034 Uiso 0.50 1 calc PR C 2
C29 C 0.08852(16) -0.23318(13) 0.26585(14) 0.0228(3) Uani 1 1 d . . .
C30 C 0.0103(2) -0.23613(17) 0.32499(17) 0.0335(4) Uani 1 1 d . C .
H30 H 0.0242 -0.1628 0.3659 0.040 Uiso 1 1 calc R . .
C31 C -0.0884(2) -0.34942(19) 0.32226(19) 0.0410(4) Uani 1 1 d . . .
H31 H -0.1451 -0.3554 0.3604 0.049 Uiso 1 1 calc R C .
C32 C -0.1036(2) -0.45416(17) 0.26320(18) 0.0389(4) Uani 1 1 d . C .
H32 H -0.1710 -0.5329 0.2597 0.047 Uiso 1 1 calc R . .
C33 C -0.0187(2) -0.44121(15) 0.20980(16) 0.0347(4) Uani 1 1 d . . .
H33 H -0.0275 -0.5130 0.1713 0.042 Uiso 1 1 calc R C .
N11 N 0.07617(16) -0.33231(12) 0.20904(12) 0.0281(3) Uani 1 1 d . C .
Fe1 Fe 0.5000 0.5000 0.5000 0.01742(8) Uani 1 2 d S . .
N13 N 0.34244(15) 0.34423(12) 0.49052(12) 0.0248(3) Uani 1 1 d . . .
C34 C 0.24199(17) 0.25613(14) 0.48147(13) 0.0232(3) Uani 1 1 d . . .
S1 S 0.10005(5) 0.13201(4) 0.46791(4) 0.03393(11) Uani 1 1 d . . .
O1W O -0.0194(3) 0.3006(2) 0.3253(3) 0.1192(11) 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 113.59(12) . . ?
N1 C1 N2 126.91(12) . . ?
N1 C1 N4 116.44(12) . . ?
N2 C1 N4 116.57(12) . . ?
C1 N2 C2 113.27(12) . . ?
N2 C2 N3 126.24(13) . . ?
N2 C2 N7 118.10(12) . . ?
N3 C2 N7 115.67(12) . . ?
C2 N3 C3 113.47(12) . . ?
N1 C3 N3 126.24(13) . . ?
N1 C3 N10 117.04(13) . . ?
N3 C3 N10 116.72(12) . . ?
C1 N4 C4 121.21(11) . . ?
C1 N4 C9 120.76(11) . . ?
C4 N4 C9 118.03(11) . . ?
N4 C4 C5 120.17(13) . . ?
N4 C4 N5 116.65(13) . . ?
C5 C4 N5 123.11(13) . . ?
C4 C5 C6 118.42(15) . . ?
C5 C6 C7 119.19(16) . . ?
C6 C7 C8 118.68(15) . . ?
C4 N5 C8 117.20(14) . . ?
C4 N5 Fe1 122.97(10) . . ?
C8 N5 Fe1 119.80(11) . . ?
C7 C8 N5 123.29(16) . . ?
N4 C9 C10 119.86(13) . . ?
N4 C9 N6 116.49(13) . . ?
C10 C9 N6 123.60(13) . . ?
C9 C10 C11 118.38(15) . . ?
C10 C11 C12 118.92(16) . . ?
C11 C12 C13 119.10(15) . . ?
C12 C13 N6 122.88(16) . . ?
C9 N6 C13 116.99(14) . . ?
C9 N6 Fe1 122.86(10) . . ?
C13 N6 Fe1 120.13(11) . . ?
C2 N7 C14 124.02(12) . . ?
C2 N7 C19 118.83(12) . . ?
C14 N7 C19 116.73(12) . . ?
N7 C14 C15 122.05(13) . . ?
N7 C14 N8 114.26(13) . . ?
C15 C14 N8 123.65(14) . . ?
C14 C15 C16 117.97(15) . . ?
C15 C16 C17 119.46(15) . . ?
C16 C17 C18 118.06(15) . . ?
C17 C18 N8 123.71(15) . . ?
C14 N8 C18 117.05(14) . . ?
N7 C19 C20 120.16(14) . . ?
N7 C19 N9 115.17(14) . . ?
C20 C19 N9 124.66(14) . . ?
C19 C20 C21 117.70(17) . . ?
C20 C21 C22 118.89(18) . . ?
C21 C22 C23 118.85(16) . . ?
C22 C23 N9 123.67(17) . . ?
C19 N9 C23 116.19(15) . . ?
C3 N10 C24 122.11(12) . . ?
C3 N10 C29 121.17(12) . . ?
C24 N10 C29 116.62(12) . . ?
N10 C24 C25A 119.29(14) . . ?
N10 C24 N12A 116.30(14) . . ?
C25A C24 N12A 124.37(15) . . ?
C27 C26 C25A 120.77(19) . . ?
C26 C27 C28 118.50(17) . . ?
C27 C28 N12A 122.31(17) . . ?
C24 C25A C26 117.21(17) . . ?
C24 N12A C28 116.80(16) . . ?
N10 C29 C30 120.87(14) . . ?
N10 C29 N11 115.06(13) . . ?
C30 C29 N11 123.97(14) . . ?
C29 C30 C31 117.82(17) . . ?
C30 C31 C32 119.24(17) . . ?
C31 C32 C33 118.42(16) . . ?
C32 C33 N11 123.63(17) . . ?
C29 N11 C33 116.88(15) . . ?
N5 Fe1 N5 180.000(1) . 2_666 ?
N5 Fe1 N6 85.50(5) . . ?
N5 Fe1 N6 94.50(5) 2_666 . ?
N5 Fe1 N6 85.50(5) 2_666 2_666 ?
N5 Fe1 N6 94.50(5) . 2_666 ?
N5 Fe1 N13 91.23(5) . . ?
N5 Fe1 N13 91.23(5) 2_666 2_666 ?
N5 Fe1 N13 88.77(5) 2_666 . ?
N5 Fe1 N13 88.77(5) . 2_666 ?
N6 Fe1 N6 180.0 . 2_666 ?
N6 Fe1 N13 91.59(5) . . ?
N6 Fe1 N13 88.41(5) . 2_666 ?
N6 Fe1 N13 91.59(5) 2_666 2_666 ?
N6 Fe1 N13 88.41(5) 2_666 . ?
N13 Fe1 N13 180.0 . 2_666 ?
Fe1 N13 C34 174.33(13) . . ?
N13 C34 S1 179.66(17) . . ?
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 1.3349(18) . ?
N1 C3 1.3408(18) . ?
C1 N2 1.3406(18) . ?
C1 N4 1.3874(17) . ?
N2 C2 1.3411(18) . ?
C2 N3 1.3486(18) . ?
C2 N7 1.3815(18) . ?
N3 C3 1.3424(18) . ?
C3 N10 1.3801(18) . ?
N4 C4 1.4257(18) . ?
N4 C9 1.4334(18) . ?
C4 C5 1.392(2) . ?
C4 N5 1.3463(19) . ?
C5 C6 1.392(2) . ?
C6 C7 1.389(3) . ?
C7 C8 1.377(3) . ?
N5 C8 1.3601(19) . ?
N5 Fe1 2.0310(13) . ?
C9 C10 1.390(2) . ?
C9 N6 1.3462(19) . ?
C10 C11 1.390(2) . ?
C11 C12 1.390(3) . ?
C12 C13 1.382(3) . ?
C13 N6 1.3610(19) . ?
N6 Fe1 2.0381(13) . ?
N7 C14 1.4285(18) . ?
N7 C19 1.4448(18) . ?
C14 C15 1.392(2) . ?
C14 N8 1.336(2) . ?
C15 C16 1.386(2) . ?
C16 C17 1.391(2) . ?
C17 C18 1.380(2) . ?
C18 N8 1.350(2) . ?
C19 C20 1.390(2) . ?
C19 N9 1.327(2) . ?
C20 C21 1.387(2) . ?
C21 C22 1.379(3) . ?
C22 C23 1.378(3) . ?
C23 N9 1.349(2) . ?
N10 C24 1.4364(19) . ?
N10 C29 1.4320(18) . ?
C24 C25A 1.368(2) . ?
C24 N12A 1.347(2) . ?
C26 C27 1.373(3) . ?
C26 C25A 1.385(3) . ?
C27 C28 1.377(3) . ?
C28 N12A 1.370(3) . ?
C29 C30 1.392(2) . ?
C29 N11 1.330(2) . ?
C30 C31 1.384(2) . ?
C31 C32 1.387(3) . ?
C32 C33 1.375(3) . ?
C33 N11 1.348(2) . ?
Fe1 N5 2.0309(13) 2_666 ?
Fe1 N6 2.0381(13) 2_666 ?
Fe1 N13 1.9802(14) . ?
Fe1 N13 1.9802(14) 2_666 ?
N13 C34 1.169(2) . ?
C34 S1 1.6455(16) . ?
