#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:08:15 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179881 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/77/7017753.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_7017753
loop_
_publ_author_name
'Klingele, Julia'
'Kaase, Dominic'
'Klingele, Marco H.'
'Lach, Jochen'
_publ_section_title
;
 Synthesis and mononuclear complexes of the bis-bidentate ligand
 2,5-di(2-pyridyl)-1,3,4-thiadiazole (dptd): spin crossover in
 [Fe(II)(dptd)2(NCSe)2] and [Fe(II)(dptd)2(NCBH3)2]·H2O.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1397
_journal_page_last               1406
_journal_paper_doi               10.1039/c1dt11396h
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety
;
C26 H22 B2 Fe N10 S2, (C H2 Cl2), (H2 O)
;
_chemical_formula_sum            'C27 H26 B2 Cl2 Fe N10 O S2'
_chemical_formula_weight         719.07
_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                76.17(3)
_cell_angle_beta                 73.65(3)
_cell_angle_gamma                67.19(3)
_cell_formula_units_Z            1
_cell_length_a                   7.5525(15)
_cell_length_b                   9.7374(19)
_cell_length_c                   12.919(3)
_cell_measurement_reflns_used    3788
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.99
_cell_volume                     831.3(4)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku R-Axis SPIDER'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0789
_diffrn_reflns_av_sigmaI/netI    0.0616
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_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            17103
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    0.779
_exptl_absorpt_correction_T_max  0.8350
_exptl_absorpt_correction_T_min  0.7614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
March 2001 T Higashi
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.752
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3788
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.1107
_refine_ls_R_factor_gt           0.0747
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1294P)²+0.2001P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2058
_refine_ls_wR_factor_ref         0.2346
_reflns_number_gt                2419
_reflns_number_total             3788
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt11396h.txt
_cod_data_source_block           jmk162
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        831.3(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7017753
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 0.5000 0.5000 0.5000 0.0426(3) Uani 1 2 d S . .
S1 S 0.31582(17) 0.81952(13) 0.21272(10) 0.0523(4) Uani 1 1 d . . .
N1 N 0.6139(5) 0.6666(4) 0.4522(3) 0.0432(8) Uani 1 1 d . . .
N2 N 0.3806(5) 0.6060(4) 0.3717(3) 0.0436(8) Uani 1 1 d . . .
N3 N 0.2601(5) 0.5769(4) 0.3235(3) 0.0444(8) Uani 1 1 d . . .
N4 N 0.0545(6) 0.8001(5) 0.0931(4) 0.0615(11) Uani 1 1 d . . .
C1 C 0.7380(6) 0.6960(6) 0.4960(4) 0.0492(11) Uani 1 1 d . . .
H1 H 0.7862 0.6274 0.5560 0.059 Uiso 1 1 calc R . .
C2 C 0.7964(7) 0.8177(6) 0.4588(4) 0.0585(12) Uani 1 1 d . . .
H2 H 0.8850 0.8313 0.4917 0.070 Uiso 1 1 calc R . .
C3 C 0.7258(8) 0.9234(6) 0.3715(5) 0.0693(15) Uani 1 1 d . . .
H3 H 0.7639 1.0098 0.3448 0.083 Uiso 1 1 calc R . .
C4 C 0.5989(8) 0.8973(6) 0.3259(5) 0.0648(14) Uani 1 1 d . . .
H4 H 0.5467 0.9661 0.2671 0.078 Uiso 1 1 calc R . .
C5 C 0.5490(6) 0.7689(5) 0.3673(4) 0.0489(11) Uani 1 1 d . . .
C6 C 0.4201(6) 0.7282(5) 0.3235(4) 0.0479(10) Uani 1 1 d . . .
C7 C 0.2141(6) 0.6800(5) 0.2408(4) 0.0440(10) Uani 1 1 d . . .
C8 C 0.0835(6) 0.6844(5) 0.1730(3) 0.0443(10) Uani 1 1 d . . .
C9 C -0.0003(7) 0.5757(6) 0.1937(4) 0.0567(12) Uani 1 1 d . . .
H9 H 0.0233 0.4947 0.2519 0.068 Uiso 1 1 calc R . .
C10 C -0.1235(7) 0.5899(6) 0.1243(4) 0.0626(13) Uani 1 1 d . . .
H10 H -0.1842 0.5171 0.1349 0.075 Uiso 1 1 calc R . .
C11 C -0.1547(7) 0.7076(6) 0.0429(4) 0.0593(13) Uani 1 1 d . . .
H11 H -0.2381 0.7191 -0.0039 0.071 Uiso 1 1 calc R . .
C12 C -0.0641(9) 0.8094(6) 0.0293(5) 0.0664(14) Uani 1 1 d . . .
H12 H -0.0859 0.8914 -0.0284 0.080 Uiso 1 1 calc R . .
N51 N 0.2778(5) 0.6302(4) 0.5890(3) 0.0465(9) Uani 1 1 d . . .
C51 C 0.1443(6) 0.7145(5) 0.6372(4) 0.0469(10) Uani 1 1 d . . .
B51 B -0.0376(8) 0.8334(7) 0.7000(5) 0.0636(16) Uani 1 1 d . . .
H51A H -0.0829 0.9256 0.6491 0.095 Uiso 1 1 calc R . .
H51B H 0.0007 0.8568 0.7584 0.095 Uiso 1 1 calc R . .
H51C H -0.1439 0.7921 0.7315 0.095 Uiso 1 1 calc R . .
Cl61 Cl 0.5756(4) 1.1414(4) 0.0883(2) 0.0792(9) Uani 0.50 1 d P A 1
Cl62 Cl 0.5383(4) 1.4493(4) 0.0523(3) 0.0850(9) Uani 0.50 1 d P . 1
C61 C 0.5584(10) 1.2775(9) 0.1515(7) 0.046(2) Uani 0.50 1 d P A 1
H61A H 0.6762 1.2481 0.1823 0.055 Uiso 0.50 1 calc PR A 1
H61B H 0.4413 1.2949 0.2120 0.055 Uiso 0.50 1 calc PR A 1
O70 O 0.5508(10) 1.2916(9) 0.2027(7) 0.166(7) Uani 0.50 1 d PR A 2
H71 H 0.5828 1.2435 0.1335 0.199 Uiso 0.50 1 d PR A 2
H72 H 0.6561 1.3379 0.1929 0.199 Uiso 0.50 1 d PR A 2
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'
B B 0.0013 0.0007 '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'
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
N51 Fe1 N51 180.0 2_666 .
N51 Fe1 N2 88.87(15) 2_666 2_666
N51 Fe1 N2 91.13(15) . 2_666
N51 Fe1 N2 91.13(15) 2_666 .
N51 Fe1 N2 88.87(15) . .
N2 Fe1 N2 180.0 2_666 .
N51 Fe1 N1 88.52(14) 2_666 2_666
N51 Fe1 N1 91.48(14) . 2_666
N2 Fe1 N1 80.49(14) 2_666 2_666
N2 Fe1 N1 99.51(15) . 2_666
N51 Fe1 N1 91.48(14) 2_666 .
N51 Fe1 N1 88.52(14) . .
N2 Fe1 N1 99.51(15) 2_666 .
N2 Fe1 N1 80.49(15) . .
N1 Fe1 N1 180.000(1) 2_666 .
C6 S1 C7 86.1(2) . .
C5 N1 C1 115.5(4) . .
C5 N1 Fe1 114.7(3) . .
C1 N1 Fe1 129.7(3) . .
C6 N2 N3 112.9(4) . .
C6 N2 Fe1 114.8(3) . .
N3 N2 Fe1 132.2(3) . .
C7 N3 N2 110.8(4) . .
C8 N4 C12 117.3(4) . .
C2 C1 N1 123.8(5) . .
C1 C2 C3 120.0(5) . .
C4 C3 C2 117.6(5) . .
C3 C4 C5 118.9(5) . .
N1 C5 C4 124.3(4) . .
N1 C5 C6 112.2(4) . .
C4 C5 C6 123.5(5) . .
N2 C6 C5 117.5(4) . .
N2 C6 S1 114.5(4) . .
C5 C6 S1 127.9(4) . .
N3 C7 C8 124.6(4) . .
N3 C7 S1 115.6(3) . .
C8 C7 S1 119.7(4) . .
N4 C8 C9 123.9(4) . .
N4 C8 C7 115.0(4) . .
C9 C8 C7 121.1(4) . .
C8 C9 C10 116.9(5) . .
C11 C10 C9 119.8(5) . .
C10 C11 C12 118.7(5) . .
N4 C12 C11 123.5(5) . .
C51 N51 Fe1 176.1(4) . .
N51 C51 B51 178.2(5) . .
Cl62 Cl62 C61 148.3(5) 2_685 .
Cl61 C61 Cl62 108.4(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N51 1.925(4) 2_666
Fe1 N51 1.925(4) .
Fe1 N2 1.982(4) 2_666
Fe1 N2 1.982(4) .
Fe1 N1 2.014(4) 2_666
Fe1 N1 2.014(4) .
S1 C6 1.716(5) .
S1 C7 1.727(4) .
N1 C5 1.356(6) .
N1 C1 1.365(6) .
N2 C6 1.307(6) .
N2 N3 1.379(5) .
N3 C7 1.302(6) .
N4 C8 1.327(6) .
N4 C12 1.344(7) .
C1 C2 1.357(7) .
C2 C3 1.405(8) .
C3 C4 1.382(7) .
C4 C5 1.386(7) .
C5 C6 1.463(6) .
C7 C8 1.477(6) .
C8 C9 1.371(7) .
C9 C10 1.414(7) .
C10 C11 1.353(8) .
C11 C12 1.362(8) .
N51 C51 1.152(5) .
C51 B51 1.573(7) .
Cl61 C61 1.662(9) .
Cl62 Cl62 1.579(7) 2_685
Cl62 C61 1.832(9) .
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
N51 Fe1 N1 C5 95.0(3) 2_666
N51 Fe1 N1 C5 -85.0(3) .
N2 Fe1 N1 C5 -175.9(3) 2_666
N2 Fe1 N1 C5 4.1(3) .
N51 Fe1 N1 C1 -88.8(4) 2_666
N51 Fe1 N1 C1 91.2(4) .
N2 Fe1 N1 C1 0.3(4) 2_666
N2 Fe1 N1 C1 -179.7(4) .
N51 Fe1 N2 C6 -94.3(3) 2_666
N51 Fe1 N2 C6 85.7(3) .
N1 Fe1 N2 C6 177.0(3) 2_666
N1 Fe1 N2 C6 -3.0(3) .
N51 Fe1 N2 N3 86.7(3) 2_666
N51 Fe1 N2 N3 -93.3(3) .
N1 Fe1 N2 N3 -2.0(4) 2_666
N1 Fe1 N2 N3 178.0(4) .
C6 N2 N3 C7 -0.3(5) .
Fe1 N2 N3 C7 178.8(3) .
C5 N1 C1 C2 -0.4(6) .
Fe1 N1 C1 C2 -176.5(3) .
N1 C1 C2 C3 1.1(7) .
C1 C2 C3 C4 -0.7(8) .
C2 C3 C4 C5 -0.5(9) .
C1 N1 C5 C4 -0.8(6) .
Fe1 N1 C5 C4 175.9(4) .
C1 N1 C5 C6 178.9(3) .
Fe1 N1 C5 C6 -4.4(4) .
C3 C4 C5 N1 1.3(8) .
C3 C4 C5 C6 -178.4(5) .
N3 N2 C6 C5 -179.3(3) .
Fe1 N2 C6 C5 1.5(5) .
N3 N2 C6 S1 -0.7(5) .
Fe1 N2 C6 S1 -179.88(18) .
N1 C5 C6 N2 2.0(6) .
C4 C5 C6 N2 -178.3(4) .
N1 C5 C6 S1 -176.4(3) .
C4 C5 C6 S1 3.3(7) .
C7 S1 C6 N2 1.0(3) .
C7 S1 C6 C5 179.5(4) .
N2 N3 C7 C8 -178.5(3) .
N2 N3 C7 S1 1.1(4) .
C6 S1 C7 N3 -1.2(3) .
C6 S1 C7 C8 178.4(3) .
C12 N4 C8 C9 -0.2(7) .
C12 N4 C8 C7 -179.7(4) .
N3 C7 C8 N4 179.5(4) .
S1 C7 C8 N4 -0.1(5) .
N3 C7 C8 C9 -0.1(6) .
S1 C7 C8 C9 -179.6(3) .
N4 C8 C9 C10 0.3(7) .
C7 C8 C9 C10 179.9(4) .
C8 C9 C10 C11 -0.5(7) .
C9 C10 C11 C12 0.6(8) .
C8 N4 C12 C11 0.2(8) .
C10 C11 C12 N4 -0.5(8) .
Cl62 Cl62 C61 Cl61 33.5(9) 2_685
