#------------------------------------------------------------------------------
#$Date: 2015-12-09 17:05:27 +0200 (Wed, 09 Dec 2015) $
#$Revision: 171266 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/68/7036816.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_7036816
loop_
_publ_author_name
'Książek, Maria'
'Kusz, Joachim'
'Białońska, Agata'
'Bronisz, Robert'
'Weselski, Marek'
_publ_section_title
;
 Influence of conformational changes on spin crossover properties and
 superstructure formation in 2D coordination polymers
 [Fe(hbtz)2(RCN)2](ClO4)2.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18563
_journal_page_last               18575
_journal_paper_doi               10.1039/c5dt03249k
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C22 H38 Fe N18, 2(Cl O4)'
_chemical_formula_sum            'C22 H38 Cl2 Fe N18 O8'
_chemical_formula_weight         809.45
_chemical_name_systematic
;
catena-[bis(μ₂-1,6-di(tetrazol-2-yl)hexane)-bis(propionitrile)]
-iron(II) diperchlorate
;
_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
_audit_update_record
;
2012-02-19 deposited with the CCDC.
2015-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90.08(3)
_cell_angle_beta                 68.46(4)
_cell_angle_gamma                66.12(3)
_cell_formula_units_Z            1
_cell_length_a                   9.403(3)
_cell_length_b                   9.602(2)
_cell_length_c                   11.546(4)
_cell_measurement_reflns_used    4671
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.55
_cell_measurement_theta_min      2.86
_cell_volume                     872.7(6)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_structure_refinement
;
SHELXL-97 (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)
;
_computing_structure_solution
;
SHELXS-97 (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)
;
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Kuma KM4CCD'
_diffrn_measurement_method       'ω scan'
_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  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0352
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7396
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.87
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.657
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.865
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            pale-pink
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3754
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0445P)²+0.0776P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0801
_reflns_number_gt                2933
_reflns_number_total             3754
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt03249k2.cif
_cod_data_source_block           3_160_down
_cod_depositor_comments
'Adding full bibliography for 7036814--7036817.cif.'
_cod_original_cell_volume        872.8(6)
_cod_database_code               7036816
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 0.5000 0.0000 0.01909(10) Uani 1 2 d S . .
Cl1 Cl 0.30030(5) 0.93878(5) 0.24461(4) 0.02853(12) Uani 1 1 d . . .
O1 O 0.2269(6) 0.9698(8) 0.1495(4) 0.0462(12) Uani 0.726(19) 1 d PU A 1
O2 O 0.4750(5) 0.9101(6) 0.1847(8) 0.0401(12) Uani 0.726(19) 1 d PU A 1
O3 O 0.2918(7) 0.8007(7) 0.2889(7) 0.0418(11) Uani 0.726(19) 1 d PU A 1
O4 O 0.2058(8) 1.0669(6) 0.3449(6) 0.0502(13) Uani 0.726(19) 1 d PU A 1
O11 O 0.2524(17) 1.0133(17) 0.1556(12) 0.045(2) Uani 0.274(19) 1 d PU A 2
O12 O 0.4661(15) 0.9317(15) 0.2308(15) 0.035(2) Uani 0.274(19) 1 d PU A 2
O13 O 0.3092(19) 0.7914(18) 0.2450(16) 0.041(2) Uani 0.274(19) 1 d PU A 2
O14 O 0.1807(17) 1.0312(18) 0.3703(13) 0.041(2) Uani 0.274(19) 1 d PU A 2
N1 N 0.1318(2) 0.03326(19) -0.12588(16) 0.0347(4) Uani 1 1 d . . .
N2 N 0.09846(18) 0.10740(17) -0.21669(14) 0.0266(3) Uani 1 1 d . . .
N3 N 0.04760(18) 0.25693(17) -0.19351(14) 0.0263(3) Uani 1 1 d . . .
N4 N 0.04639(17) 0.28510(17) -0.07982(13) 0.0246(3) Uani 1 1 d . . .
C1 C 0.1301(2) 0.0255(2) -0.33734(18) 0.0322(4) Uani 1 1 d . . .
H1A H 0.0757 0.1007 -0.3841 0.039 Uiso 1 1 calc R . .
H1B H 0.0790 -0.0485 -0.3210 0.039 Uiso 1 1 calc R . .
C2 C 0.3194(2) -0.0612(2) -0.41696(18) 0.0320(4) Uani 1 1 d . . .
H2A H 0.3372 -0.1231 -0.4940 0.038 Uiso 1 1 calc R . .
H2B H 0.3730 -0.1339 -0.3684 0.038 Uiso 1 1 calc R . .
C3 C 0.4069(2) 0.0444(2) -0.45615(18) 0.0307(4) Uani 1 1 d . . .
H3A H 0.3482 0.1223 -0.4993 0.037 Uiso 1 1 calc R . .
H3B H 0.3975 0.1003 -0.3796 0.037 Uiso 1 1 calc R . .
C4 C 0.0976(2) 0.1480(2) -0.04174(18) 0.0313(4) Uani 1 1 d . . .
H4 H 0.1081 0.1351 0.0368 0.038 Uiso 1 1 calc R . .
N11 N -0.36443(19) 0.54565(18) 0.36453(15) 0.0304(4) Uani 1 1 d . . .
N12 N -0.22090(17) 0.43225(16) 0.36206(14) 0.0233(3) Uani 1 1 d . . .
N13 N -0.09130(18) 0.39220(16) 0.25211(14) 0.0257(3) Uani 1 1 d . . .
N14 N -0.15139(18) 0.48187(16) 0.17769(14) 0.0244(3) Uani 1 1 d . . .
C11 C -0.2041(2) 0.3701(2) 0.47422(17) 0.0262(4) Uani 1 1 d . . .
H11A H -0.0922 0.2799 0.4491 0.031 Uiso 1 1 calc R . .
H11B H -0.2933 0.3347 0.5145 0.031 Uiso 1 1 calc R . .
C12 C -0.2206(2) 0.4928(2) 0.56858(17) 0.0285(4) Uani 1 1 d . . .
H12A H -0.2083 0.4470 0.6431 0.034 Uiso 1 1 calc R . .
H12B H -0.3363 0.5787 0.5978 0.034 Uiso 1 1 calc R . .
C13 C -0.0913(2) 0.5593(2) 0.51667(17) 0.0265(4) Uani 1 1 d . . .
H13A H -0.1000 0.6014 0.4400 0.032 Uiso 1 1 calc R . .
H13B H -0.1201 0.6461 0.5805 0.032 Uiso 1 1 calc R . .
C14 C -0.3166(2) 0.5729(2) 0.24828(17) 0.0283(4) Uani 1 1 d . . .
H14 H -0.3902 0.6482 0.2176 0.034 Uiso 1 1 calc R . .
N20 N 0.2079(2) 0.39721(17) 0.04208(14) 0.0278(3) Uani 1 1 d . . .
C20 C 0.3179(2) 0.3325(2) 0.07167(16) 0.0278(4) Uani 1 1 d . . .
C21 C 0.4568(2) 0.2519(2) 0.11083(18) 0.0323(4) Uani 1 1 d . . .
H21A H 0.5253 0.1451 0.0621 0.039 Uiso 1 1 calc R . .
H21B H 0.4092 0.2453 0.2015 0.039 Uiso 1 1 calc R . .
C22 C 0.5717(3) 0.3332(3) 0.0905(2) 0.0430(5) Uani 1 1 d . . .
H22A H 0.6632 0.2752 0.1178 0.064 Uiso 1 1 calc R . .
H22B H 0.5050 0.4382 0.1401 0.064 Uiso 1 1 calc R . .
H22C H 0.6208 0.3385 0.0006 0.064 Uiso 1 1 calc R . .
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'
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'
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
N20 Fe1 N20 180.00(13) 2_565 .
N20 Fe1 N4 89.31(7) 2_565 2_565
N20 Fe1 N4 90.69(7) . 2_565
N20 Fe1 N4 90.69(7) 2_565 .
N20 Fe1 N4 89.31(7) . .
N4 Fe1 N4 180.0 2_565 .
N20 Fe1 N14 89.48(7) 2_565 2_565
N20 Fe1 N14 90.52(7) . 2_565
N4 Fe1 N14 92.38(7) 2_565 2_565
N4 Fe1 N14 87.62(7) . 2_565
N20 Fe1 N14 90.52(7) 2_565 .
N20 Fe1 N14 89.48(7) . .
N4 Fe1 N14 87.62(7) 2_565 .
N4 Fe1 N14 92.38(7) . .
N14 Fe1 N14 180.00(8) 2_565 .
O11 Cl1 O13 115.4(7) . .
O11 Cl1 O4 97.4(5) . .
O13 Cl1 O4 128.7(5) . .
O11 Cl1 O2 96.0(5) . .
O13 Cl1 O2 103.0(6) . .
O4 Cl1 O2 111.9(3) . .
O11 Cl1 O3 130.5(6) . .
O13 Cl1 O3 18.9(6) . .
O4 Cl1 O3 111.0(2) . .
O2 Cl1 O3 108.8(3) . .
O11 Cl1 O14 109.1(7) . .
O13 Cl1 O14 107.9(6) . .
O4 Cl1 O14 20.9(5) . .
O2 Cl1 O14 125.5(5) . .
O3 Cl1 O14 90.6(5) . .
O11 Cl1 O1 23.0(6) . .
O13 Cl1 O1 93.3(6) . .
O4 Cl1 O1 109.0(3) . .
O2 Cl1 O1 108.5(3) . .
O3 Cl1 O1 107.6(3) . .
O14 Cl1 O1 113.2(6) . .
O11 Cl1 O12 109.9(6) . .
O13 Cl1 O12 109.2(8) . .
O4 Cl1 O12 93.7(5) . .
O2 Cl1 O12 21.1(4) . .
O3 Cl1 O12 107.8(5) . .
O14 Cl1 O12 104.9(7) . .
O1 Cl1 O12 126.7(5) . .
C4 N1 N2 101.61(15) . .
N3 N2 N1 114.70(15) . .
N3 N2 C1 122.91(15) . .
N1 N2 C1 122.21(15) . .
N2 N3 N4 104.99(14) . .
N3 N4 C4 106.44(15) . .
N3 N4 Fe1 122.88(11) . .
C4 N4 Fe1 130.28(13) . .
N2 C1 C2 110.63(15) . .
N2 C1 H1A 109.5 . .
C2 C1 H1A 109.5 . .
N2 C1 H1B 109.5 . .
C2 C1 H1B 109.5 . .
H1A C1 H1B 108.1 . .
C1 C2 C3 113.42(15) . .
C1 C2 H2A 108.9 . .
C3 C2 H2A 108.9 . .
C1 C2 H2B 108.9 . .
C3 C2 H2B 108.9 . .
H2A C2 H2B 107.7 . .
C3 C3 C2 112.20(19) 2_654 .
C3 C3 H3A 109.2 2_654 .
C2 C3 H3A 109.2 . .
C3 C3 H3B 109.2 2_654 .
C2 C3 H3B 109.2 . .
H3A C3 H3B 107.9 . .
N1 C4 N4 112.25(17) . .
N1 C4 H4 123.9 . .
N4 C4 H4 123.9 . .
C14 N11 N12 102.05(15) . .
N13 N12 N11 113.76(15) . .
N13 N12 C11 122.65(14) . .
N11 N12 C11 123.27(15) . .
N12 N13 N14 105.41(14) . .
N13 N14 C14 106.58(15) . .
N13 N14 Fe1 124.00(11) . .
C14 N14 Fe1 128.42(13) . .
N12 C11 C12 110.64(14) . .
N12 C11 H11A 109.5 . .
C12 C11 H11A 109.5 . .
N12 C11 H11B 109.5 . .
C12 C11 H11B 109.5 . .
H11A C11 H11B 108.1 . .
C11 C12 C13 114.60(15) . .
C11 C12 H12A 108.6 . .
C13 C12 H12A 108.6 . .
C11 C12 H12B 108.6 . .
C13 C12 H12B 108.6 . .
H12A C12 H12B 107.6 . .
C13 C13 C12 113.37(18) 2_566 .
C13 C13 H13A 108.9 2_566 .
C12 C13 H13A 108.9 . .
C13 C13 H13B 108.9 2_566 .
C12 C13 H13B 108.9 . .
H13A C13 H13B 107.7 . .
N11 C14 N14 112.20(17) . .
N11 C14 H14 123.9 . .
N14 C14 H14 123.9 . .
C20 N20 Fe1 174.20(14) . .
N20 C20 C21 179.19(19) . .
C20 C21 C22 112.23(16) . .
C20 C21 H21A 109.2 . .
C22 C21 H21A 109.2 . .
C20 C21 H21B 109.2 . .
C22 C21 H21B 109.2 . .
H21A C21 H21B 107.9 . .
C21 C22 H22A 109.5 . .
C21 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C21 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N20 2.0413(18) 2_565
Fe1 N20 2.0414(18) .
Fe1 N4 2.0660(16) 2_565
Fe1 N4 2.0660(16) .
Fe1 N14 2.0792(18) 2_565
Fe1 N14 2.0792(18) .
Cl1 O11 1.362(12) .
Cl1 O13 1.384(17) .
Cl1 O4 1.414(5) .
Cl1 O2 1.433(4) .
Cl1 O3 1.443(6) .
Cl1 O14 1.465(13) .
Cl1 O1 1.470(5) .
Cl1 O12 1.481(12) .
N1 C4 1.320(2) .
N1 N2 1.329(2) .
N2 N3 1.308(2) .
N2 C1 1.467(2) .
N3 N4 1.335(2) .
N4 C4 1.342(2) .
C1 C2 1.517(3) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 C3 1.521(3) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C3 1.519(4) 2_654
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 H4 0.9500 .
N11 C14 1.313(2) .
N11 N12 1.338(2) .
N12 N13 1.314(2) .
N12 C11 1.461(2) .
N13 N14 1.328(2) .
N14 C14 1.345(2) .
C11 C12 1.524(2) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 C13 1.530(2) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 C13 1.524(3) 2_566
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 H14 0.9500 .
N20 C20 1.146(2) .
C20 C21 1.458(3) .
C21 C22 1.527(3) .
C21 H21A 0.9900 .
C21 H21B 0.9900 .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
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
C4 N1 N2 N3 0.2(2) . .
C4 N1 N2 C1 175.34(15) . .
N1 N2 N3 N4 -0.13(19) . .
C1 N2 N3 N4 -175.27(14) . .
N2 N3 N4 C4 0.03(18) . .
N2 N3 N4 Fe1 173.52(10) . .
N20 Fe1 N4 N3 48.15(13) 2_565 .
N20 Fe1 N4 N3 -131.85(13) . .
N4 Fe1 N4 N3 173(85) 2_565 .
N14 Fe1 N4 N3 -41.30(13) 2_565 .
N14 Fe1 N4 N3 138.70(13) . .
N20 Fe1 N4 C4 -140.05(16) 2_565 .
N20 Fe1 N4 C4 39.95(16) . .
N4 Fe1 N4 C4 -15(85) 2_565 .
N14 Fe1 N4 C4 130.50(16) 2_565 .
N14 Fe1 N4 C4 -49.50(16) . .
N3 N2 C1 C2 104.04(19) . .
N1 N2 C1 C2 -70.7(2) . .
N2 C1 C2 C3 -63.9(2) . .
C1 C2 C3 C3 -175.6(2) . 2_654
N2 N1 C4 N4 -0.1(2) . .
N3 N4 C4 N1 0.1(2) . .
Fe1 N4 C4 N1 -172.76(12) . .
C14 N11 N12 N13 0.67(19) . .
C14 N11 N12 C11 174.28(15) . .
N11 N12 N13 N14 -0.56(18) . .
C11 N12 N13 N14 -174.21(14) . .
N12 N13 N14 C14 0.20(17) . .
N12 N13 N14 Fe1 169.58(10) . .
N20 Fe1 N14 N13 164.93(13) 2_565 .
N20 Fe1 N14 N13 -15.07(13) . .
N4 Fe1 N14 N13 -105.79(14) 2_565 .
N4 Fe1 N14 N13 74.21(14) . .
N14 Fe1 N14 N13 -45(100) 2_565 .
N20 Fe1 N14 C14 -28.10(15) 2_565 .
N20 Fe1 N14 C14 151.90(15) . .
N4 Fe1 N14 C14 61.18(15) 2_565 .
N4 Fe1 N14 C14 -118.82(15) . .
N14 Fe1 N14 C14 122(100) 2_565 .
N13 N12 C11 C12 107.57(17) . .
N11 N12 C11 C12 -65.5(2) . .
N12 C11 C12 C13 -58.1(2) . .
C11 C12 C13 C13 -65.3(3) . 2_566
N12 N11 C14 N14 -0.52(19) . .
N13 N14 C14 N11 0.2(2) . .
Fe1 N14 C14 N11 -168.54(12) . .
N20 Fe1 N20 C20 60(100) 2_565 .
N4 Fe1 N20 C20 120.4(14) 2_565 .
N4 Fe1 N20 C20 -59.6(14) . .
N14 Fe1 N20 C20 -147.3(14) 2_565 .
N14 Fe1 N20 C20 32.7(14) . .
Fe1 N20 C20 C21 -93(15) . .
N20 C20 C21 C22 -70(15) . .
