#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:31:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179451 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/48/4334899.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_4334899
loop_
_publ_author_name
'Julia Klingele'
'Dominic Kaase'
'Maximilian Schmucker'
'Yanhua Lan'
'Guillaume Chastanet'
'Jean-François Létard'
_publ_contact_author             'Julia Klingele'
_publ_contact_author_email       julia.klingele@ac.uni-freiburg.de
_publ_section_title
;
 Thermal Spin Crossover and LIESST Effect Observed in Complexes
 [Fe(LCh)2(NCX)2] [LCh= 2,5-Di(2-Pyridyl)-1,3,4-Chalcadiazole; Ch = O, S,
 Se; X = S, Se, BH3]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6000
_journal_page_last               6010
_journal_paper_doi               10.1021/ic400342m
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety
;
 (Fe C26 H16 N10 O2 S2)
;
_chemical_formula_sum            'C26 H16 Fe N10 O2 S2'
_chemical_formula_weight         620.46
_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                 95.8981(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.5518(2)
_cell_length_b                   7.7916(2)
_cell_length_c                   17.7393(3)
_cell_measurement_reflns_used    6206
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.5
_cell_measurement_theta_min      2.3
_cell_volume                     1313.24(5)
_computing_data_collection       'Bruker APEX2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Bruker APEX2 CCD area detector'
_diffrn_measurement_method       'f\ and ω scans'
_diffrn_radiation_monochromator  'multilayer mirror optics'
_diffrn_radiation_source         'microfused sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20856
_diffrn_reflns_theta_full        34.85
_diffrn_reflns_theta_max         34.85
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    0.780
_exptl_absorpt_correction_T_max  0.9846
_exptl_absorpt_correction_T_min  0.9260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         5417
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0347
_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)+(0.0374P)²+0.5155P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0877
_reflns_number_gt                4294
_reflns_number_total             5417
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400342m_si_004.cif
_cod_data_source_block           dk_ms27
_cod_database_code               4334899
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
Fe1 Fe 0.0000 0.5000 0.0000 0.01207(6) Uani 1 2 d S
N1 N 0.04714(11) 0.68580(13) 0.09394(6) 0.01382(18) Uani 1 1 d .
N2 N -0.13564(11) 0.72717(13) -0.03401(6) 0.01407(19) Uani 1 1 d .
N3 N -0.23627(11) 0.78762(14) -0.09092(6) 0.01527(19) Uani 1 1 d .
N4 N -0.42288(12) 1.02976(14) -0.17490(6) 0.0167(2) Uani 1 1 d .
O1 O -0.21450(9) 0.97407(11) 0.00431(5) 0.01401(16) Uani 1 1 d .
C1 C 0.13361(13) 0.66114(16) 0.15701(7) 0.0163(2) Uani 1 1 d .
H1 H 0.1914 0.5617 0.1606 0.020 Uiso 1 1 calc R
C2 C 0.14273(13) 0.77481(17) 0.21779(7) 0.0173(2) Uani 1 1 d .
H2 H 0.2058 0.7534 0.2617 0.021 Uiso 1 1 calc R
C3 C 0.05844(14) 0.91957(17) 0.21320(7) 0.0183(2) Uani 1 1 d .
H3 H 0.0629 0.9988 0.2541 0.022 Uiso 1 1 calc R
C4 C -0.03300(14) 0.94814(17) 0.14808(7) 0.0171(2) Uani 1 1 d .
H4 H -0.0921 1.0464 0.1434 0.021 Uiso 1 1 calc R
C5 C -0.03453(12) 0.82811(15) 0.09049(7) 0.0133(2) Uani 1 1 d .
C6 C -0.12695(12) 0.84009(15) 0.01986(7) 0.0131(2) Uani 1 1 d .
C7 C -0.27974(12) 0.93258(16) -0.06589(7) 0.0134(2) Uani 1 1 d .
C8 C -0.38749(12) 1.05126(15) -0.10021(7) 0.0137(2) Uani 1 1 d .
C9 C -0.44680(13) 1.17236(16) -0.05573(7) 0.0168(2) Uani 1 1 d .
H9 H -0.4166 1.1832 -0.0032 0.020 Uiso 1 1 calc R
C10 C -0.55209(14) 1.27738(17) -0.09077(8) 0.0211(3) Uani 1 1 d .
H10 H -0.5949 1.3630 -0.0627 0.025 Uiso 1 1 calc R
C11 C -0.59334(14) 1.25489(17) -0.16722(8) 0.0213(3) Uani 1 1 d .
H11 H -0.6664 1.3229 -0.1923 0.026 Uiso 1 1 calc R
C12 C -0.52575(14) 1.13084(17) -0.20649(8) 0.0195(2) Uani 1 1 d .
H12 H -0.5544 1.1170 -0.2590 0.023 Uiso 1 1 calc R
N50 N 0.15628(12) 0.59484(15) -0.06007(7) 0.0190(2) Uani 1 1 d .
C50 C 0.23483(13) 0.65163(15) -0.09961(7) 0.0147(2) Uani 1 1 d .
S50 S 0.34624(4) 0.73357(4) -0.15282(2) 0.01994(7) 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
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
H H 0.0000 0.0000 '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
N50 Fe1 N50 180.00(5) 3_565 .
N50 Fe1 N1 86.98(4) 3_565 .
N50 Fe1 N1 93.02(4) . .
N50 Fe1 N1 93.02(4) 3_565 3_565
N50 Fe1 N1 86.98(4) . 3_565
N1 Fe1 N1 180.0 . 3_565
N50 Fe1 N2 90.40(4) 3_565 3_565
N50 Fe1 N2 89.60(4) . 3_565
N1 Fe1 N2 104.26(4) . 3_565
N1 Fe1 N2 75.74(4) 3_565 3_565
N50 Fe1 N2 89.60(4) 3_565 .
N50 Fe1 N2 90.40(4) . .
N1 Fe1 N2 75.74(4) . .
N1 Fe1 N2 104.26(4) 3_565 .
N2 Fe1 N2 180.0 3_565 .
C1 N1 C5 117.39(11) . .
C1 N1 Fe1 126.59(8) . .
C5 N1 Fe1 115.41(8) . .
C6 N2 N3 106.87(10) . .
C6 N2 Fe1 110.28(8) . .
N3 N2 Fe1 142.60(8) . .
C7 N3 N2 105.42(10) . .
C12 N4 C8 116.08(11) . .
C6 O1 C7 102.56(9) . .
N1 C1 C2 122.83(12) . .
C3 C2 C1 118.93(11) . .
C2 C3 C4 119.39(12) . .
C5 C4 C3 117.55(12) . .
N1 C5 C4 123.91(11) . .
N1 C5 C6 112.72(10) . .
C4 C5 C6 123.37(11) . .
N2 C6 O1 112.56(10) . .
N2 C6 C5 125.24(11) . .
O1 C6 C5 122.20(10) . .
N3 C7 O1 112.59(10) . .
N3 C7 C8 129.91(11) . .
O1 C7 C8 117.47(10) . .
N4 C8 C9 124.71(11) . .
N4 C8 C7 115.14(11) . .
C9 C8 C7 120.14(11) . .
C8 C9 C10 117.65(12) . .
C11 C10 C9 118.87(13) . .
C10 C11 C12 118.65(12) . .
N4 C12 C11 124.00(12) . .
C50 N50 Fe1 173.53(11) . .
N50 C50 S50 178.49(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N50 2.0583(12) 3_565
Fe1 N50 2.0583(12) .
Fe1 N1 2.2184(10) .
Fe1 N1 2.2185(10) 3_565
Fe1 N2 2.2394(10) 3_565
Fe1 N2 2.2394(10) .
N1 C1 1.3345(15) .
N1 C5 1.3535(15) .
N2 C6 1.2953(16) .
N2 N3 1.4019(14) .
N3 C7 1.2973(16) .
N4 C12 1.3367(16) .
N4 C8 1.3437(16) .
O1 C6 1.3482(14) .
O1 C7 1.3725(14) .
C1 C2 1.3911(18) .
C2 C3 1.3833(19) .
C3 C4 1.3926(18) .
C4 C5 1.3841(17) .
C5 C6 1.4596(16) .
C7 C8 1.4685(16) .
C8 C9 1.3877(18) .
C9 C10 1.3924(17) .
C10 C11 1.384(2) .
C11 C12 1.389(2) .
N50 C50 1.1657(17) .
C50 S50 1.6240(13) .
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
N50 Fe1 N1 C1 87.49(11) 3_565
N50 Fe1 N1 C1 -92.51(11) .
N2 Fe1 N1 C1 -2.16(11) 3_565
N2 Fe1 N1 C1 177.84(11) .
N50 Fe1 N1 C5 -83.31(9) 3_565
N50 Fe1 N1 C5 96.69(9) .
N2 Fe1 N1 C5 -172.96(8) 3_565
N2 Fe1 N1 C5 7.04(8) .
N50 Fe1 N2 C6 81.37(9) 3_565
N50 Fe1 N2 C6 -98.63(9) .
N1 Fe1 N2 C6 -5.62(8) .
N1 Fe1 N2 C6 174.38(8) 3_565
N50 Fe1 N2 N3 -91.79(14) 3_565
N50 Fe1 N2 N3 88.21(14) .
N1 Fe1 N2 N3 -178.78(14) .
N1 Fe1 N2 N3 1.22(14) 3_565
C6 N2 N3 C7 -0.15(13) .
Fe1 N2 N3 C7 173.15(11) .
C5 N1 C1 C2 -0.29(19) .
Fe1 N1 C1 C2 -170.92(9) .
N1 C1 C2 C3 0.3(2) .
C1 C2 C3 C4 -0.1(2) .
C2 C3 C4 C5 -0.04(19) .
C1 N1 C5 C4 0.13(18) .
Fe1 N1 C5 C4 171.82(10) .
C1 N1 C5 C6 -178.72(11) .
Fe1 N1 C5 C6 -7.04(13) .
C3 C4 C5 N1 0.0(2) .
C3 C4 C5 C6 178.76(12) .
N3 N2 C6 O1 0.10(14) .
Fe1 N2 C6 O1 -175.57(8) .
N3 N2 C6 C5 179.86(11) .
Fe1 N2 C6 C5 4.20(15) .
C7 O1 C6 N2 -0.01(13) .
C7 O1 C6 C5 -179.78(11) .
N1 C5 C6 N2 1.82(18) .
C4 C5 C6 N2 -177.05(12) .
N1 C5 C6 O1 -178.44(11) .
C4 C5 C6 O1 2.69(19) .
N2 N3 C7 O1 0.15(14) .
N2 N3 C7 C8 -178.14(12) .
C6 O1 C7 N3 -0.10(13) .
C6 O1 C7 C8 178.43(10) .
C12 N4 C8 C9 -2.02(19) .
C12 N4 C8 C7 176.80(11) .
N3 C7 C8 N4 -17.6(2) .
O1 C7 C8 N4 164.15(11) .
N3 C7 C8 C9 161.25(13) .
O1 C7 C8 C9 -16.98(17) .
N4 C8 C9 C10 1.0(2) .
C7 C8 C9 C10 -177.72(12) .
C8 C9 C10 C11 0.8(2) .
C9 C10 C11 C12 -1.5(2) .
C8 N4 C12 C11 1.25(19) .
C10 C11 C12 N4 0.4(2) .
