#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/49/4334900.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_4334900
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 S2 Se2), 1.4(C H2 Cl2), 0.6(C H4 O)
;
_chemical_formula_sum            'C28 H21.2 Cl2.8 Fe N10 O0.6 S2 Se2'
_chemical_formula_weight         884.50
_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                90.506(2)
_cell_angle_beta                 105.465(2)
_cell_angle_gamma                103.219(2)
_cell_formula_units_Z            1
_cell_length_a                   7.5704(2)
_cell_length_b                   9.2523(3)
_cell_length_c                   12.5256(4)
_cell_measurement_reflns_used    3036
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.6
_cell_measurement_theta_min      2.3
_cell_volume                     820.89(4)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0583
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18189
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    3.073
_exptl_absorpt_correction_T_max  0.9135
_exptl_absorpt_correction_T_min  0.7487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_description       block
_exptl_crystal_F_000             438
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.832
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         4056
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0407
_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)+(0.0440P)²+0.9171P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0986
_reflns_number_gt                3156
_reflns_number_total             4056
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400342m_si_005.cif
_cod_data_source_block           jmk_dk24_1
_cod_original_formula_sum        'C28 H21.20 Cl2.80 Fe N10 O0.60 S2 Se2'
_cod_database_code               4334900
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
Fe1 Fe 0.0000 0.0000 1.0000 0.01716(15) Uani 1 2 d S . .
N1 N -0.1413(4) 0.1630(3) 0.9805(2) 0.0194(6) Uani 1 1 d . . .
N2 N 0.1028(4) 0.1100(3) 0.8863(2) 0.0198(6) Uani 1 1 d . . .
N3 N 0.2301(4) 0.0816(3) 0.8338(2) 0.0207(6) Uani 1 1 d . . .
N4 N 0.4278(4) 0.2935(3) 0.6377(2) 0.0236(6) Uani 1 1 d . . .
Se1 Se 0.15358(5) 0.33828(4) 0.75808(3) 0.02211(11) Uani 1 1 d . . .
C1 C -0.2695(5) 0.1853(4) 1.0308(3) 0.0256(7) Uani 1 1 d . . .
H1 H -0.3060 0.1154 1.0807 0.031 Uiso 1 1 calc R . .
C2 C -0.3514(5) 0.3060(4) 1.0133(3) 0.0266(8) Uani 1 1 d . . .
H2 H -0.4412 0.3177 1.0511 0.032 Uiso 1 1 calc R . .
C3 C -0.3020(5) 0.4083(4) 0.9413(3) 0.0241(7) Uani 1 1 d . . .
H3 H -0.3570 0.4913 0.9282 0.029 Uiso 1 1 calc R . .
C4 C -0.1706(5) 0.3878(4) 0.8881(3) 0.0232(7) Uani 1 1 d . . .
H4 H -0.1340 0.4564 0.8375 0.028 Uiso 1 1 calc R . .
C5 C -0.0929(4) 0.2657(3) 0.9098(3) 0.0188(6) Uani 1 1 d . . .
C6 C 0.0454(4) 0.2315(4) 0.8589(3) 0.0200(7) Uani 1 1 d . . .
C7 C 0.2727(4) 0.1815(3) 0.7671(3) 0.0189(6) Uani 1 1 d . . .
C8 C 0.4069(4) 0.1782(4) 0.7017(3) 0.0196(6) Uani 1 1 d . . .
C9 C 0.5015(5) 0.0663(4) 0.7073(3) 0.0239(7) Uani 1 1 d . . .
H9 H 0.4813 -0.0131 0.7536 0.029 Uiso 1 1 calc R . .
C10 C 0.6264(5) 0.0727(4) 0.6435(3) 0.0263(7) Uani 1 1 d . . .
H10 H 0.6942 -0.0023 0.6453 0.032 Uiso 1 1 calc R . .
C11 C 0.6510(5) 0.1906(4) 0.5769(3) 0.0283(8) Uani 1 1 d . . .
H11 H 0.7354 0.1976 0.5320 0.034 Uiso 1 1 calc R . .
C12 C 0.5493(5) 0.2986(4) 0.5773(3) 0.0266(7) Uani 1 1 d . . .
H12 H 0.5677 0.3798 0.5324 0.032 Uiso 1 1 calc R . .
C50 C 0.3066(5) 0.2172(4) 1.1799(3) 0.0220(7) Uani 1 1 d . . .
N50 N 0.1981(4) 0.1294(3) 1.1143(2) 0.0204(6) Uani 1 1 d . . .
S50 S 0.46275(15) 0.34180(11) 1.27258(8) 0.0373(2) Uani 1 1 d . . .
C60 C 0.9943(16) 0.2907(10) 0.3584(8) 0.052(3) Uani 0.50 1 d PD A 1
H60A H 0.8697 0.2744 0.3029 0.062 Uiso 0.50 1 calc PR A 1
H60B H 1.0930 0.3204 0.3191 0.062 Uiso 0.50 1 calc PR A 1
Cl61 Cl 1.0168(5) 0.1191(5) 0.4231(5) 0.122(2) Uani 0.50 1 d PD A 1
Cl62 Cl 1.0176(4) 0.4391(3) 0.4609(2) 0.0688(8) Uani 0.50 1 d PD . 1
C70 C 1.1006(19) 0.2374(17) 0.4200(15) 0.030(4) Uani 0.20 1 d PD B 2
H70A H 1.1615 0.3123 0.4839 0.037 Uiso 0.20 1 calc PR B 2
H70B H 1.1927 0.2346 0.3773 0.037 Uiso 0.20 1 calc PR B 2
Cl71 Cl 1.0232(8) 0.0540(5) 0.4687(4) 0.0191(9) Uani 0.20 1 d PD . 2
Cl72 Cl 0.8933(8) 0.2843(5) 0.3329(4) 0.0300(11) Uani 0.20 1 d PD B 2
O80 O 1.0898 0.4007 0.3164 0.006 Uani 0.15 1 d P C 3
H80 H 1.1461 0.3963 0.3834 0.009 Uiso 0.15 1 calc PR C 3
C80 C 0.9384 0.2767 0.2818 0.050 Uani 0.15 1 d P C 3
H80A H 0.9824 0.1860 0.3008 0.075 Uiso 0.15 1 calc PR C 3
H80B H 0.8846 0.2737 0.2012 0.075 Uiso 0.15 1 calc PR C 3
H80C H 0.8417 0.2832 0.3191 0.075 Uiso 0.15 1 calc PR C 3
O85 O 0.9605 0.2304 0.3210 0.021 Uani 0.15 1 d P D 4
H85 H 0.9563 0.2699 0.2606 0.031 Uiso 0.15 1 d P E 4
C85 C 1.0294 0.3591 0.4219 0.050 Uani 0.15 1 d P D 4
H85A H 0.9189 0.3831 0.4377 0.075 Uiso 0.15 1 d P F 4
H85B H 1.1065 0.4484 0.4007 0.075 Uiso 0.15 1 d P G 4
H85C H 1.1045 0.3237 0.4883 0.075 Uiso 0.15 1 d P H 4
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'
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'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
N50 Fe1 N50 180.0 . 2_557
N50 Fe1 N2 90.90(11) . 2_557
N50 Fe1 N2 89.10(11) 2_557 2_557
N50 Fe1 N2 89.10(11) . .
N50 Fe1 N2 90.90(11) 2_557 .
N2 Fe1 N2 180.00(14) 2_557 .
N50 Fe1 N1 88.29(11) . .
N50 Fe1 N1 91.71(11) 2_557 .
N2 Fe1 N1 100.01(11) 2_557 .
N2 Fe1 N1 79.99(11) . .
N50 Fe1 N1 91.71(11) . 2_557
N50 Fe1 N1 88.29(11) 2_557 2_557
N2 Fe1 N1 79.99(11) 2_557 2_557
N2 Fe1 N1 100.01(11) . 2_557
N1 Fe1 N1 180.00(15) . 2_557
C1 N1 C5 116.7(3) . .
C1 N1 Fe1 128.6(2) . .
C5 N1 Fe1 114.7(2) . .
C6 N2 N3 114.5(3) . .
C6 N2 Fe1 115.5(2) . .
N3 N2 Fe1 130.0(2) . .
C7 N3 N2 113.5(3) . .
C12 N4 C8 116.9(3) . .
C6 Se1 C7 81.56(14) . .
N1 C1 C2 123.0(3) . .
C3 C2 C1 119.7(3) . .
C2 C3 C4 118.5(3) . .
C3 C4 C5 119.0(3) . .
N1 C5 C4 123.1(3) . .
N1 C5 C6 112.6(3) . .
C4 C5 C6 124.2(3) . .
N2 C6 C5 117.0(3) . .
N2 C6 Se1 114.7(2) . .
C5 C6 Se1 128.3(2) . .
N3 C7 C8 124.3(3) . .
N3 C7 Se1 115.8(2) . .
C8 C7 Se1 119.9(2) . .
N4 C8 C9 124.2(3) . .
N4 C8 C7 113.8(3) . .
C9 C8 C7 122.1(3) . .
C8 C9 C10 118.2(3) . .
C9 C10 C11 118.9(3) . .
C10 C11 C12 118.6(3) . .
N4 C12 C11 123.2(3) . .
N50 C50 S50 179.3(3) . .
C50 N50 Fe1 173.3(3) . .
Cl61 C60 Cl62 111.2(5) . .
Cl62 Cl62 C60 165.7(5) 2_766 .
Cl72 C70 Cl71 107.1(8) . .
Cl71 Cl71 C70 163.0(9) 2_756 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N50 1.933(3) .
Fe1 N50 1.933(3) 2_557
Fe1 N2 1.982(3) 2_557
Fe1 N2 1.982(3) .
Fe1 N1 2.021(3) .
Fe1 N1 2.021(3) 2_557
N1 C1 1.341(4) .
N1 C5 1.360(4) .
N2 C6 1.312(4) .
N2 N3 1.371(4) .
N3 C7 1.294(4) .
N4 C12 1.331(4) .
N4 C8 1.346(4) .
Se1 C6 1.856(3) .
Se1 C7 1.865(3) .
C1 C2 1.388(5) .
C2 C3 1.373(5) .
C3 C4 1.380(5) .
C4 C5 1.386(4) .
C5 C6 1.452(4) .
C7 C8 1.471(4) .
C8 C9 1.379(5) .
C9 C10 1.383(5) .
C10 C11 1.388(5) .
C11 C12 1.395(5) .
C50 N50 1.154(4) .
C50 S50 1.642(4) .
C60 Cl61 1.811(10) .
C60 Cl62 1.816(8) .
Cl62 Cl62 1.601(6) 2_766
C70 Cl72 1.802(12) .
C70 Cl71 1.830(12) .
Cl71 Cl71 1.319(8) 2_756
O80 C80 1.3937 .
O85 C85 1.6200 .
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
_geom_torsion_site_symmetry_4
N50 Fe1 N1 C1 -91.4(3) . .
N50 Fe1 N1 C1 88.6(3) 2_557 .
N2 Fe1 N1 C1 -0.8(3) 2_557 .
N2 Fe1 N1 C1 179.2(3) . .
N50 Fe1 N1 C5 85.8(2) . .
N50 Fe1 N1 C5 -94.2(2) 2_557 .
N2 Fe1 N1 C5 176.4(2) 2_557 .
N2 Fe1 N1 C5 -3.6(2) . .
N50 Fe1 N2 C6 -84.7(2) . .
N50 Fe1 N2 C6 95.3(2) 2_557 .
N1 Fe1 N2 C6 3.7(2) . .
N1 Fe1 N2 C6 -176.3(2) 2_557 .
N50 Fe1 N2 N3 93.0(3) . .
N50 Fe1 N2 N3 -87.0(3) 2_557 .
N1 Fe1 N2 N3 -178.6(3) . .
N1 Fe1 N2 N3 1.4(3) 2_557 .
C6 N2 N3 C7 0.8(4) . .
Fe1 N2 N3 C7 -176.9(2) . .
C5 N1 C1 C2 0.1(5) . .
Fe1 N1 C1 C2 177.3(3) . .
N1 C1 C2 C3 0.4(6) . .
C1 C2 C3 C4 -0.2(5) . .
C2 C3 C4 C5 -0.4(5) . .
C1 N1 C5 C4 -0.6(5) . .
Fe1 N1 C5 C4 -178.2(3) . .
C1 N1 C5 C6 -179.6(3) . .
Fe1 N1 C5 C6 2.8(3) . .
C3 C4 C5 N1 0.8(5) . .
C3 C4 C5 C6 179.6(3) . .
N3 N2 C6 C5 178.6(3) . .
Fe1 N2 C6 C5 -3.3(4) . .
N3 N2 C6 Se1 -1.3(4) . .
Fe1 N2 C6 Se1 176.77(14) . .
N1 C5 C6 N2 0.3(4) . .
C4 C5 C6 N2 -178.6(3) . .
N1 C5 C6 Se1 -179.8(2) . .
C4 C5 C6 Se1 1.2(5) . .
C7 Se1 C6 N2 1.0(2) . .
C7 Se1 C6 C5 -178.9(3) . .
N2 N3 C7 C8 179.4(3) . .
N2 N3 C7 Se1 0.0(4) . .
C6 Se1 C7 N3 -0.6(2) . .
C6 Se1 C7 C8 -179.9(3) . .
C12 N4 C8 C9 -0.7(5) . .
C12 N4 C8 C7 179.1(3) . .
N3 C7 C8 N4 179.6(3) . .
Se1 C7 C8 N4 -1.1(4) . .
N3 C7 C8 C9 -0.7(5) . .
Se1 C7 C8 C9 178.6(3) . .
N4 C8 C9 C10 0.3(5) . .
C7 C8 C9 C10 -179.4(3) . .
C8 C9 C10 C11 -0.1(5) . .
C9 C10 C11 C12 0.3(5) . .
C8 N4 C12 C11 0.9(5) . .
C10 C11 C12 N4 -0.8(5) . .
Cl61 C60 Cl62 Cl62 -102.8(17) . 2_766
Cl72 C70 Cl71 Cl71 -106(3) . 2_756
