#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:56:49 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180364 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/33/7203353.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_7203353
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                95.223(2)
_cell_angle_beta                 111.650(2)
_cell_angle_gamma                116.420(2)
_cell_formula_units_Z            1
_cell_length_a                   11.7103(5)
_cell_length_b                   12.8096(6)
_cell_length_c                   12.9408(6)
_cell_measurement_reflns_used    6872
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.548
_cell_measurement_theta_min      2.319
_cell_volume                     1537.99(13)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.965
_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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0446
_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            17506
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.59
_diffrn_reflns_theta_min         2.32
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.386
_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    1.496
_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         0.559
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         9033
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0434
_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)+(0.0625P)²+0.4509P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1206
_reflns_number_gt                7565
_reflns_number_total             9033
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b602903e.txt
_cod_data_source_block           eu_22_01a
_cod_original_cell_volume        1537.98(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7203353
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 0.27815(13) 0.08506(10) 0.27450(10) 0.0156(2) Uani 1 1 d . . .
C1 C 0.24050(14) 0.16595(12) 0.24268(11) 0.0130(2) Uani 1 1 d . . .
N2 N 0.10747(12) 0.14556(10) 0.18822(10) 0.0149(2) Uani 1 1 d . . .
C2 C 0.00543(15) 0.02846(12) 0.16119(12) 0.0142(2) Uani 1 1 d . . .
N3 N 0.02664(13) -0.06476(10) 0.17924(11) 0.0158(2) Uani 1 1 d . . .
C3 C 0.16567(15) -0.02905(12) 0.23925(12) 0.0145(2) Uani 1 1 d . . .
N4 N 0.35272(12) 0.28573(10) 0.27561(10) 0.0137(2) Uani 1 1 d . . .
C4 C 0.32586(14) 0.37972(12) 0.24553(12) 0.0141(2) Uani 1 1 d . . .
C5 C 0.24582(15) 0.36633(13) 0.12927(12) 0.0167(3) Uani 1 1 d . . .
H5 H 0.2056 0.2934 0.0693 0.020 Uiso 1 1 calc R . .
C6 C 0.22598(16) 0.46138(14) 0.10261(13) 0.0203(3) Uani 1 1 d . . .
H6 H 0.1689 0.4535 0.0244 0.024 Uiso 1 1 calc R . .
C7 C 0.29109(17) 0.56874(14) 0.19239(14) 0.0210(3) Uani 1 1 d . . .
H7 H 0.2806 0.6357 0.1763 0.025 Uiso 1 1 calc R . .
N5 N 0.38680(13) 0.48169(10) 0.33368(10) 0.0144(2) Uani 1 1 d . . .
C8 C 0.37105(16) 0.57574(13) 0.30491(13) 0.0183(3) Uani 1 1 d . . .
H8 H 0.4175 0.6499 0.3654 0.022 Uiso 1 1 calc R . .
C9 C 0.49857(14) 0.31854(12) 0.34055(12) 0.0139(2) Uani 1 1 d . . .
C10 C 0.55212(16) 0.25699(13) 0.29775(13) 0.0185(3) Uani 1 1 d . . .
H10 H 0.4921 0.1924 0.2260 0.022 Uiso 1 1 calc R . .
C11 C 0.69489(17) 0.29174(14) 0.36195(14) 0.0219(3) Uani 1 1 d . . .
H11 H 0.7331 0.2487 0.3370 0.026 Uiso 1 1 calc R . .
C12 C 0.78091(16) 0.39097(14) 0.46377(14) 0.0213(3) Uani 1 1 d . . .
H12 H 0.8794 0.4177 0.5086 0.026 Uiso 1 1 calc R . .
C13 C 0.72092(15) 0.45004(13) 0.49867(13) 0.0182(3) Uani 1 1 d . . .
H13 H 0.7811 0.5195 0.5665 0.022 Uiso 1 1 calc R . .
N6 N 0.57949(12) 0.41309(10) 0.44010(10) 0.0146(2) Uani 1 1 d . . .
N7 N -0.13635(13) -0.00196(11) 0.10961(11) 0.0165(2) Uani 1 1 d . . .
C14 C -0.18184(15) 0.08205(12) 0.07830(12) 0.0158(3) Uani 1 1 d . . .
C15 C -0.11693(15) 0.16998(14) 0.03008(12) 0.0180(3) Uani 1 1 d . . .
H15 H -0.0417 0.1749 0.0147 0.022 Uiso 1 1 calc R . .
C16 C -0.16593(17) 0.25000(14) 0.00531(13) 0.0213(3) Uani 1 1 d . . .
H16 H -0.1225 0.3125 -0.0254 0.026 Uiso 1 1 calc R . .
C17 C -0.27928(17) 0.23774(14) 0.02586(14) 0.0225(3) Uani 1 1 d . . .
H17 H -0.3135 0.2923 0.0110 0.027 Uiso 1 1 calc R . .
C18 C -0.34043(17) 0.14373(14) 0.06857(14) 0.0224(3) Uani 1 1 d . . .
H18 H -0.4206 0.1329 0.0793 0.027 Uiso 1 1 calc R . .
N8 N -0.29292(14) 0.06674(12) 0.09583(12) 0.0211(3) Uani 1 1 d . . .
C19 C -0.24505(15) -0.12086(12) 0.10045(13) 0.0162(3) Uani 1 1 d . . .
C20 C -0.24455(17) -0.15108(15) 0.20139(14) 0.0223(3) Uani 1 1 d . . .
H20 H -0.1738 -0.0946 0.2767 0.027 Uiso 1 1 calc R . .
C21 C -0.35127(19) -0.26684(16) 0.18788(16) 0.0275(3) Uani 1 1 d . . .
H21 H -0.3551 -0.2914 0.2542 0.033 Uiso 1 1 calc R . .
C22 C -0.45184(18) -0.34563(15) 0.07613(16) 0.0268(3) Uani 1 1 d . . .
H22 H -0.5247 -0.4259 0.0644 0.032 Uiso 1 1 calc R . .
C23 C -0.44427(17) -0.30533(14) -0.01815(15) 0.0250(3) Uani 1 1 d . . .
H23 H -0.5149 -0.3594 -0.0945 0.030 Uiso 1 1 calc R . .
N9 N -0.34217(14) -0.19358(12) -0.00769(11) 0.0208(3) Uani 1 1 d . . .
N10 N 0.19607(13) -0.11850(11) 0.26698(11) 0.0171(2) Uani 1 1 d . C .
C24 C 0.33756(15) -0.09916(12) 0.30555(12) 0.0156(3) Uani 1 1 d . . .
C26 C 0.5472(2) -0.03534(16) 0.28453(18) 0.0317(4) Uani 1 1 d . . .
H26 H 0.6020 -0.0020 0.2446 0.038 Uiso 1 1 calc R A 1
C27 C 0.60315(18) -0.06816(16) 0.38116(18) 0.0340(4) Uani 1 1 d . C .
H27 H 0.6964 -0.0568 0.4088 0.041 Uiso 1 1 calc R . .
C28 C 0.5206(2) -0.11782(15) 0.43671(15) 0.0304(4) Uani 1 1 d . . .
H28 H 0.5586 -0.1404 0.5034 0.036 Uiso 1 1 calc R B 1
C25A C 0.41228(17) -0.05051(13) 0.24530(14) 0.0234(3) Uani 0.50 1 d P C 1
H25A H 0.3730 -0.0280 0.1790 0.028 Uiso 0.50 1 calc PR C 1
N12A N 0.38584(16) -0.13559(12) 0.39898(12) 0.0212(3) Uani 0.50 1 d P C 1
N12B N 0.41228(17) -0.05051(13) 0.24530(14) 0.0234(3) Uani 0.50 1 d P C 2
C25B C 0.38584(16) -0.13559(12) 0.39898(12) 0.0212(3) Uani 0.50 1 d P C 2
H25B H 0.3288 -0.1718 0.4366 0.025 Uiso 0.50 1 calc PR C 2
C29 C 0.08861(15) -0.23235(13) 0.26519(13) 0.0168(3) Uani 1 1 d . . .
C30 C 0.00987(19) -0.23500(15) 0.32470(15) 0.0249(3) Uani 1 1 d . C .
H30 H 0.0235 -0.1615 0.3653 0.030 Uiso 1 1 calc R . .
C31 C -0.0891(2) -0.34859(17) 0.32265(17) 0.0303(4) Uani 1 1 d . . .
H31 H -0.1464 -0.3544 0.3606 0.036 Uiso 1 1 calc R C .
C32 C -0.10324(19) -0.45357(16) 0.26428(16) 0.0288(4) Uani 1 1 d . C .
H32 H -0.1707 -0.5324 0.2610 0.035 Uiso 1 1 calc R . .
C33 C -0.01678(19) -0.44040(14) 0.21121(14) 0.0252(3) Uani 1 1 d . . .
H33 H -0.0244 -0.5121 0.1737 0.030 Uiso 1 1 calc R C .
N11 N 0.07770(14) -0.33170(11) 0.20955(11) 0.0203(3) Uani 1 1 d . C .
Fe1 Fe 0.5000 0.5000 0.5000 0.01254(8) Uani 1 2 d S . .
N13 N 0.34365(13) 0.34559(11) 0.48966(10) 0.0167(2) Uani 1 1 d . . .
C34 C 0.24420(15) 0.25725(13) 0.48133(12) 0.0162(3) Uani 1 1 d . . .
S1 S 0.10249(4) 0.13246(3) 0.46833(3) 0.02366(10) Uani 1 1 d . . .
O1W O -0.0224(2) 0.2996(2) 0.3285(2) 0.0886(8) 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 127.14(12) . . ?
N1 C1 N4 116.02(12) . . ?
N2 C1 N4 116.75(11) . . ?
C1 N2 C2 113.14(11) . . ?
N2 C2 N3 126.39(13) . . ?
N2 C2 N7 118.11(12) . . ?
N3 C2 N7 115.50(12) . . ?
C2 N3 C3 113.37(11) . . ?
N1 C3 N3 126.30(12) . . ?
N1 C3 N10 116.80(12) . . ?
N3 C3 N10 116.91(12) . . ?
C1 N4 C4 121.10(11) . . ?
C1 N4 C9 121.11(11) . . ?
C4 N4 C9 117.79(11) . . ?
N4 C4 C5 120.29(12) . . ?
N4 C4 N5 116.63(12) . . ?
C5 C4 N5 123.02(12) . . ?
C4 C5 C6 118.80(13) . . ?
C5 C6 C7 118.96(13) . . ?
C6 C7 C8 118.68(13) . . ?
C4 N5 C8 117.14(12) . . ?
C4 N5 Fe1 122.89(9) . . ?
C8 N5 Fe1 119.95(9) . . ?
C7 C8 N5 123.31(13) . . ?
N4 C9 C10 119.95(12) . . ?
N4 C9 N6 116.71(12) . . ?
C10 C9 N6 123.29(13) . . ?
C9 C10 C11 118.79(13) . . ?
C10 C11 C12 118.66(14) . . ?
C11 C12 C13 119.10(14) . . ?
C12 C13 N6 122.92(13) . . ?
C9 N6 C13 117.10(12) . . ?
C9 N6 Fe1 122.56(9) . . ?
C13 N6 Fe1 120.32(9) . . ?
C2 N7 C14 124.21(11) . . ?
C2 N7 C19 118.64(11) . . ?
C14 N7 C19 116.60(11) . . ?
N7 C14 C15 122.01(13) . . ?
N7 C14 N8 114.41(12) . . ?
C15 C14 N8 123.55(13) . . ?
C14 C15 C16 117.89(14) . . ?
C15 C16 C17 119.43(14) . . ?
C16 C17 C18 117.95(14) . . ?
C17 C18 N8 123.79(14) . . ?
C14 N8 C18 117.26(13) . . ?
N7 C19 C20 119.87(13) . . ?
N7 C19 N9 115.40(12) . . ?
C20 C19 N9 124.71(13) . . ?
C19 C20 C21 117.65(15) . . ?
C20 C21 C22 118.86(15) . . ?
C21 C22 C23 118.76(15) . . ?
C22 C23 N9 123.67(15) . . ?
C19 N9 C23 116.32(14) . . ?
C3 N10 C24 121.95(11) . . ?
C3 N10 C29 120.98(12) . . ?
C24 N10 C29 116.97(11) . . ?
N10 C24 C25A 119.45(13) . . ?
N10 C24 N12A 116.19(13) . . ?
C25A C24 N12A 124.32(14) . . ?
C27 C26 C25A 120.69(17) . . ?
C26 C27 C28 118.49(16) . . ?
C27 C28 N12A 122.19(16) . . ?
C24 C25A C26 117.42(15) . . ?
C24 N12A C28 116.86(15) . . ?
N10 C29 C30 120.93(13) . . ?
N10 C29 N11 114.94(12) . . ?
C30 C29 N11 124.00(14) . . ?
C29 C30 C31 117.87(15) . . ?
C30 C31 C32 119.11(16) . . ?
C31 C32 C33 118.32(15) . . ?
C32 C33 N11 123.81(15) . . ?
C29 N11 C33 116.84(14) . . ?
N5 Fe1 N5 180.0 . 2_666 ?
N5 Fe1 N6 86.24(5) . . ?
N5 Fe1 N6 93.76(5) 2_666 . ?
N5 Fe1 N6 86.24(5) 2_666 2_666 ?
N5 Fe1 N6 93.76(5) . 2_666 ?
N5 Fe1 N13 91.30(5) . . ?
N5 Fe1 N13 88.70(5) 2_666 . ?
N5 Fe1 N13 91.29(5) 2_666 2_666 ?
N5 Fe1 N13 88.71(5) . 2_666 ?
N6 Fe1 N6 180.00(6) . 2_666 ?
N6 Fe1 N13 91.71(5) . . ?
N6 Fe1 N13 88.29(5) . 2_666 ?
N6 Fe1 N13 88.29(5) 2_666 . ?
N6 Fe1 N13 91.71(5) 2_666 2_666 ?
N13 Fe1 N13 180.0 . 2_666 ?
Fe1 N13 C34 175.04(12) . . ?
N13 C34 S1 179.41(15) . . ?
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 1.3372(17) . ?
N1 C3 1.3422(17) . ?
C1 N2 1.3364(17) . ?
C1 N4 1.3915(17) . ?
N2 C2 1.3421(17) . ?
C2 N3 1.3468(17) . ?
C2 N7 1.3832(18) . ?
N3 C3 1.3426(18) . ?
C3 N10 1.3828(17) . ?
N4 C4 1.4256(17) . ?
N4 C9 1.4274(17) . ?
C4 C5 1.3931(19) . ?
C4 N5 1.3473(17) . ?
C5 C6 1.387(2) . ?
C6 C7 1.395(2) . ?
C7 C8 1.379(2) . ?
N5 C8 1.3612(17) . ?
N5 Fe1 1.9927(12) . ?
C9 C10 1.3923(19) . ?
C9 N6 1.3484(17) . ?
C10 C11 1.389(2) . ?
C11 C12 1.394(2) . ?
C12 C13 1.384(2) . ?
C13 N6 1.3609(18) . ?
N6 Fe1 2.0011(12) . ?
N7 C14 1.4270(17) . ?
N7 C19 1.4438(17) . ?
C14 C15 1.397(2) . ?
C14 N8 1.3345(19) . ?
C15 C16 1.389(2) . ?
C16 C17 1.393(2) . ?
C17 C18 1.384(2) . ?
C18 N8 1.347(2) . ?
C19 C20 1.394(2) . ?
C19 N9 1.3286(19) . ?
C20 C21 1.391(2) . ?
C21 C22 1.384(3) . ?
C22 C23 1.384(2) . ?
C23 N9 1.349(2) . ?
N10 C24 1.4345(18) . ?
N10 C29 1.4318(17) . ?
C24 C25A 1.367(2) . ?
C24 N12A 1.3536(19) . ?
C26 C27 1.381(3) . ?
C26 C25A 1.381(2) . ?
C27 C28 1.380(3) . ?
C28 N12A 1.368(2) . ?
C29 C30 1.395(2) . ?
C29 N11 1.3322(19) . ?
C30 C31 1.390(2) . ?
C31 C32 1.390(3) . ?
C32 C33 1.381(3) . ?
C33 N11 1.3474(19) . ?
Fe1 N5 1.9927(12) 2_666 ?
Fe1 N6 2.0012(12) 2_666 ?
Fe1 N13 1.9572(13) . ?
Fe1 N13 1.9572(13) 2_666 ?
N13 C34 1.1665(19) . ?
C34 S1 1.6498(15) . ?
