#------------------------------------------------------------------------------
#$Date: 2015-12-09 17:05:27 +0200 (Wed, 09 Dec 2015) $
#$Revision: 171266 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/68/7036817.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_7036817
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                90.68(3)
_cell_angle_beta                 68.74(4)
_cell_angle_gamma                66.37(3)
_cell_formula_units_Z            1
_cell_length_a                   9.341(3)
_cell_length_b                   9.555(2)
_cell_length_c                   11.409(4)
_cell_measurement_reflns_used    5183
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.73
_cell_measurement_theta_min      2.90
_cell_volume                     854.6(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      100(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  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_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            7328
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.91
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.671
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.869
_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            purple
_exptl_crystal_density_diffrn    1.573
_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         0.365
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3667
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0298
_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)+(0.0492P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0804
_reflns_number_gt                3020
_reflns_number_total             3667
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt03249k2.cif
_cod_data_source_block           3_100_down
_cod_depositor_comments
'Adding full bibliography for 7036814--7036817.cif.'
_cod_database_code               7036817
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 0.01141(10) Uani 1 2 d S . .
Cl1 Cl 0.30208(5) 0.93647(4) 0.24186(4) 0.01713(11) Uani 1 1 d . . .
O1 O 0.2276(9) 0.9641(11) 0.1462(7) 0.0242(12) Uani 0.74(4) 1 d PU A 1
O2 O 0.4787(8) 0.9088(9) 0.1803(11) 0.0215(11) Uani 0.74(4) 1 d PU A 1
O3 O 0.2935(14) 0.7959(12) 0.2893(11) 0.0231(11) Uani 0.74(4) 1 d PU A 1
O4 O 0.2095(13) 1.0679(9) 0.3442(9) 0.0277(13) Uani 0.74(4) 1 d PU A 1
O11 O 0.246(3) 0.995(3) 0.148(2) 0.028(3) Uani 0.26(4) 1 d PU A 2
O12 O 0.471(2) 0.927(2) 0.215(2) 0.020(2) Uani 0.26(4) 1 d PU A 2
O13 O 0.307(4) 0.798(4) 0.262(3) 0.027(3) Uani 0.26(4) 1 d PU A 2
O14 O 0.185(3) 1.047(3) 0.362(2) 0.023(3) Uani 0.26(4) 1 d PU A 2
N1 N 0.12659(18) 0.03947(16) -0.12343(13) 0.0190(3) Uani 1 1 d . . .
N2 N 0.09435(17) 0.11337(16) -0.21565(13) 0.0151(3) Uani 1 1 d . . .
N3 N 0.04503(17) 0.26410(15) -0.19264(13) 0.0148(3) Uani 1 1 d . . .
N4 N 0.04472(16) 0.29219(15) -0.07778(13) 0.0138(3) Uani 1 1 d . . .
C1 C 0.1259(2) 0.0299(2) -0.33784(16) 0.0182(3) Uani 1 1 d . . .
H1A H 0.0724 0.1049 -0.3856 0.022 Uiso 1 1 calc R . .
H1B H 0.0735 -0.0437 -0.3214 0.022 Uiso 1 1 calc R . .
C2 C 0.3165(2) -0.05888(19) -0.41774(16) 0.0180(3) Uani 1 1 d . . .
H2A H 0.3343 -0.1203 -0.4965 0.022 Uiso 1 1 calc R . .
H2B H 0.3689 -0.1326 -0.3687 0.022 Uiso 1 1 calc R . .
C3 C 0.4067(2) 0.04581(19) -0.45515(16) 0.0181(3) Uani 1 1 d . . .
H3A H 0.3485 0.1257 -0.4976 0.022 Uiso 1 1 calc R . .
H3B H 0.3992 0.0998 -0.3770 0.022 Uiso 1 1 calc R . .
C4 C 0.0935(2) 0.15517(19) -0.03791(16) 0.0177(3) Uani 1 1 d . . .
H4 H 0.1029 0.1431 0.0419 0.021 Uiso 1 1 calc R . .
N11 N -0.36291(17) 0.54521(16) 0.35841(13) 0.0173(3) Uani 1 1 d . . .
N12 N -0.21932(16) 0.43172(15) 0.35620(12) 0.0133(3) Uani 1 1 d . . .
N13 N -0.08714(17) 0.39248(15) 0.24618(13) 0.0148(3) Uani 1 1 d . . .
N14 N -0.14647(16) 0.48376(15) 0.17130(13) 0.0136(3) Uani 1 1 d . . .
C11 C -0.2051(2) 0.36966(18) 0.47019(15) 0.0151(3) Uani 1 1 d . . .
H11A H -0.0931 0.2787 0.4456 0.018 Uiso 1 1 calc R . .
H11B H -0.2954 0.3348 0.5096 0.018 Uiso 1 1 calc R . .
C12 C -0.2224(2) 0.49348(19) 0.56679(15) 0.0167(3) Uani 1 1 d . . .
H12A H -0.2114 0.4481 0.6424 0.020 Uiso 1 1 calc R . .
H12B H -0.3382 0.5799 0.5957 0.020 Uiso 1 1 calc R . .
C13 C -0.0916(2) 0.55962(18) 0.51597(16) 0.0162(3) Uani 1 1 d . . .
H13A H -0.0985 0.6008 0.4380 0.019 Uiso 1 1 calc R . .
H13B H -0.1213 0.6475 0.5809 0.019 Uiso 1 1 calc R . .
C14 C -0.3131(2) 0.57488(19) 0.24144(15) 0.0159(3) Uani 1 1 d . . .
H14 H -0.3860 0.6512 0.2105 0.019 Uiso 1 1 calc R . .
N20 N 0.19715(17) 0.40287(15) 0.04184(12) 0.0139(3) Uani 1 1 d . . .
C20 C 0.3071(2) 0.33860(18) 0.07230(15) 0.0144(3) Uani 1 1 d . . .
C21 C 0.4464(2) 0.25640(19) 0.11273(16) 0.0176(3) Uani 1 1 d . . .
H21A H 0.5137 0.1487 0.0637 0.021 Uiso 1 1 calc R . .
H21B H 0.3977 0.2510 0.2045 0.021 Uiso 1 1 calc R . .
C22 C 0.5649(2) 0.3355(2) 0.09264(19) 0.0247(4) Uani 1 1 d . . .
H22A H 0.6562 0.2761 0.1204 0.037 Uiso 1 1 calc R . .
H22B H 0.4997 0.4413 0.1429 0.037 Uiso 1 1 calc R . .
H22C H 0.6149 0.3399 0.0017 0.037 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(12) . 2_565
N20 Fe1 N4 90.72(6) . 2_565
N20 Fe1 N4 89.28(6) 2_565 2_565
N20 Fe1 N4 89.28(6) . .
N20 Fe1 N4 90.72(6) 2_565 .
N4 Fe1 N4 180.00(3) 2_565 .
N20 Fe1 N14 90.63(7) . 2_565
N20 Fe1 N14 89.37(7) 2_565 2_565
N4 Fe1 N14 92.24(7) 2_565 2_565
N4 Fe1 N14 87.76(7) . 2_565
N20 Fe1 N14 89.37(7) . .
N20 Fe1 N14 90.63(7) 2_565 .
N4 Fe1 N14 87.76(7) 2_565 .
N4 Fe1 N14 92.24(7) . .
N14 Fe1 N14 180.00(8) 2_565 .
O13 Cl1 O11 115.9(16) . .
O13 Cl1 O4 121.2(10) . .
O11 Cl1 O4 102.6(9) . .
O13 Cl1 O2 105.0(14) . .
O11 Cl1 O2 99.6(9) . .
O4 Cl1 O2 110.5(4) . .
O13 Cl1 O12 107.7(16) . .
O11 Cl1 O12 111.2(10) . .
O4 Cl1 O12 96.6(8) . .
O2 Cl1 O12 15.9(7) . .
O13 Cl1 O14 107.6(12) . .
O11 Cl1 O14 107.2(12) . .
O4 Cl1 O14 14.5(9) . .
O2 Cl1 O14 121.9(8) . .
O12 Cl1 O14 106.9(11) . .
O13 Cl1 O1 100.5(14) . .
O11 Cl1 O1 15.8(10) . .
O4 Cl1 O1 110.1(5) . .
O2 Cl1 O1 108.7(4) . .
O12 Cl1 O1 122.4(8) . .
O14 Cl1 O1 110.9(10) . .
O13 Cl1 O3 10.5(13) . .
O11 Cl1 O3 123.2(11) . .
O4 Cl1 O3 110.9(4) . .
O2 Cl1 O3 109.2(5) . .
O12 Cl1 O3 109.0(9) . .
O14 Cl1 O3 97.5(9) . .
O1 Cl1 O3 107.4(5) . .
C4 N1 N2 101.68(13) . .
N3 N2 N1 114.95(13) . .
N3 N2 C1 122.85(14) . .
N1 N2 C1 122.01(14) . .
N2 N3 N4 104.49(13) . .
N3 N4 C4 107.11(13) . .
N3 N4 Fe1 122.42(11) . .
C4 N4 Fe1 130.21(11) . .
N2 C1 C2 110.52(14) . .
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 113.43(14) . .
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 111.76(17) 2_654 .
C3 C3 H3A 109.3 2_654 .
C2 C3 H3A 109.3 . .
C3 C3 H3B 109.3 2_654 .
C2 C3 H3B 109.3 . .
H3A C3 H3B 107.9 . .
N1 C4 N4 111.77(15) . .
N1 C4 H4 124.1 . .
N4 C4 H4 124.1 . .
C14 N11 N12 102.12(14) . .
N13 N12 N11 114.09(14) . .
N13 N12 C11 122.68(13) . .
N11 N12 C11 122.84(13) . .
N12 N13 N14 105.04(13) . .
N13 N14 C14 106.95(13) . .
N13 N14 Fe1 124.04(11) . .
C14 N14 Fe1 128.27(12) . .
N12 C11 C12 110.40(13) . .
N12 C11 H11A 109.6 . .
C12 C11 H11A 109.6 . .
N12 C11 H11B 109.6 . .
C12 C11 H11B 109.6 . .
H11A C11 H11B 108.1 . .
C11 C12 C13 114.58(14) . .
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 113.47(17) 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 111.80(15) . .
N11 C14 H14 124.1 . .
N14 C14 H14 124.1 . .
C20 N20 Fe1 174.34(13) . .
N20 C20 C21 179.35(17) . .
C20 C21 C22 112.49(14) . .
C20 C21 H21A 109.1 . .
C22 C21 H21A 109.1 . .
C20 C21 H21B 109.1 . .
C22 C21 H21B 109.1 . .
H21A C21 H21B 107.8 . .
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 1.9387(15) .
Fe1 N20 1.9387(15) 2_565
Fe1 N4 1.9822(15) 2_565
Fe1 N4 1.9822(15) .
Fe1 N14 1.9884(17) 2_565
Fe1 N14 1.9884(17) .
Cl1 O13 1.33(3) .
Cl1 O11 1.38(2) .
Cl1 O4 1.432(8) .
Cl1 O2 1.446(7) .
Cl1 O12 1.46(2) .
Cl1 O14 1.46(2) .
Cl1 O1 1.468(8) .
Cl1 O3 1.475(11) .
N1 C4 1.323(2) .
N1 N2 1.332(2) .
N2 N3 1.3141(19) .
N2 C1 1.468(2) .
N3 N4 1.3333(19) .
N4 C4 1.347(2) .
C1 C2 1.521(2) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 C3 1.523(2) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C3 1.521(3) 2_654
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 H4 0.9500 .
N11 C14 1.320(2) .
N11 N12 1.3358(19) .
N12 N13 1.3170(19) .
N12 C11 1.463(2) .
N13 N14 1.3309(19) .
N14 C14 1.347(2) .
C11 C12 1.525(2) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 C13 1.531(2) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 C13 1.528(3) 2_566
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 H14 0.9500 .
N20 C20 1.145(2) .
C20 C21 1.466(2) .
C21 C22 1.530(2) .
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 0.21(17) . .
C4 N1 N2 C1 175.27(14) . .
N1 N2 N3 N4 0.10(17) . .
C1 N2 N3 N4 -174.92(13) . .
N2 N3 N4 C4 -0.37(16) . .
N2 N3 N4 Fe1 174.36(9) . .
N20 Fe1 N4 N3 -132.55(12) . .
N20 Fe1 N4 N3 47.45(12) 2_565 .
N4 Fe1 N4 N3 92(100) 2_565 .
N14 Fe1 N4 N3 -41.89(12) 2_565 .
N14 Fe1 N4 N3 138.11(12) . .
N20 Fe1 N4 C4 40.85(15) . .
N20 Fe1 N4 C4 -139.15(14) 2_565 .
N4 Fe1 N4 C4 -94(100) 2_565 .
N14 Fe1 N4 C4 131.51(14) 2_565 .
N14 Fe1 N4 C4 -48.49(14) . .
N3 N2 C1 C2 103.85(17) . .
N1 N2 C1 C2 -70.82(19) . .
N2 C1 C2 C3 -62.84(19) . .
C1 C2 C3 C3 -174.76(17) . 2_654
N2 N1 C4 N4 -0.44(17) . .
N3 N4 C4 N1 0.53(18) . .
Fe1 N4 C4 N1 -173.64(11) . .
C14 N11 N12 N13 0.43(17) . .
C14 N11 N12 C11 173.42(14) . .
N11 N12 N13 N14 -0.51(17) . .
C11 N12 N13 N14 -173.51(13) . .
N12 N13 N14 C14 0.36(16) . .
N12 N13 N14 Fe1 171.19(9) . .
N20 Fe1 N14 N13 -16.23(12) . .
N20 Fe1 N14 N13 163.77(12) 2_565 .
N4 Fe1 N14 N13 -106.98(13) 2_565 .
N4 Fe1 N14 N13 73.02(13) . .
N14 Fe1 N14 N13 -147(100) 2_565 .
N20 Fe1 N14 C14 152.57(14) . .
N20 Fe1 N14 C14 -27.43(14) 2_565 .
N4 Fe1 N14 C14 61.82(14) 2_565 .
N4 Fe1 N14 C14 -118.18(14) . .
N14 Fe1 N14 C14 22(100) 2_565 .
N13 N12 C11 C12 106.48(16) . .
N11 N12 C11 C12 -65.91(19) . .
N12 C11 C12 C13 -57.94(18) . .
C11 C12 C13 C13 -65.6(2) . 2_566
N12 N11 C14 N14 -0.18(17) . .
N13 N14 C14 N11 -0.12(18) . .
Fe1 N14 C14 N11 -170.43(11) . .
N20 Fe1 N20 C20 -4(100) 2_565 .
N4 Fe1 N20 C20 121.0(13) 2_565 .
N4 Fe1 N20 C20 -59.0(13) . .
N14 Fe1 N20 C20 -146.8(13) 2_565 .
N14 Fe1 N20 C20 33.2(13) . .
Fe1 N20 C20 C21 -38(16) . .
N20 C20 C21 C22 -126(15) . .
