#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:38:42 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179590 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/55/4505566.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_4505566
loop_
_publ_author_name
'Liu, Wen-Ting'
'Li, Jin-Yan'
'Ni, Zhao-Ping'
'Bao, Xin'
'Ou, Yong-Cong'
'Leng, Ji-Dong'
'Liu, Jun-Liang'
'Tong, Ming-Liang'
_publ_section_title
;
 Incomplete Spin Crossover versus Antiferromagnetic Behavior Exhibited in
 Three-Dimensional Porous Fe(II)-Bis(tetrazolate) Frameworks
;
_journal_issue                   3
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1482
_journal_paper_doi               10.1021/cg201569m
_journal_volume                  12
_journal_year                    2012
_chemical_formula_sum            'C46 H80 Fe3 N24 O17'
_chemical_formula_weight         1408.89
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 110.68(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.106(2)
_cell_length_b                   24.627(3)
_cell_length_c                   12.118(2)
_cell_measurement_temperature    110(2)
_cell_volume                     3380.0(10)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type
'Goniometer Xcalibur, detector: Sapphire3 (Gemini ultra Cu)'
_diffrn_measurement_method       'ω and π scan'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1085
_diffrn_reflns_av_sigmaI/netI    0.1610
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4601
_diffrn_reflns_theta_full        61.17
_diffrn_reflns_theta_max         61.17
_diffrn_reflns_theta_min         3.59
_exptl_absorpt_coefficient_mu    5.770
_exptl_absorpt_correction_T_max  0.6247
_exptl_absorpt_correction_T_min  0.4404
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1476
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
;
_refine_diff_density_max         0.774
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.915
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         2547
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0749
_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)+(0.0685P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1774
_refine_ls_wR_factor_ref         0.1906
_reflns_number_gt                1600
_reflns_number_total             2547
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg201569m_si_001.cif
_cod_data_source_block           2.5n-BuOH(110K)
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               4505566
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
Fe1 Fe 0.5000 0.5000 0.0000 0.0161(4) Uani 1 4 d S
Fe2 Fe 0.39597(10) 0.5000 0.25705(11) 0.0217(4) Uani 1 2 d S
N1 N 0.7306(6) 0.5000 0.2120(7) 0.0375(19) Uani 1 2 d S
H1N H 0.7776 0.5000 0.1668 0.045 Uiso 0.17 2 d SPR
N2 N 0.6124(5) 0.5000 0.1757(6) 0.0224(15) Uani 1 2 d S
N3 N 0.5786(6) 0.5000 0.2648(6) 0.0284(17) Uani 1 2 d S
N4 N 0.6704(5) 0.5000 0.3645(6) 0.0320(17) Uani 1 2 d S
H4N H 0.6678 0.5000 0.4393 0.038 Uiso 0.17 2 d SPR
N5 N 0.3718(5) 0.3902(2) -0.0201(5) 0.0408(14) Uani 1 1 d .
H5N H 0.3849 0.3801 -0.0841 0.049 Uiso 0.17 1 calc PR
N6 N 0.3978(4) 0.43858(18) 0.0358(4) 0.0238(11) Uani 1 1 d .
N7 N 0.3608(4) 0.4378(2) 0.1251(5) 0.0369(13) Uani 1 1 d .
N8 N 0.3154(5) 0.3900(2) 0.1354(5) 0.0490(16) Uani 1 1 d .
H8N H 0.2831 0.3792 0.1898 0.059 Uiso 0.17 1 d PR
O1 O 0.4493(4) 0.44459(15) 0.4028(4) 0.0316(10) Uani 1 1 d .
O1W O 0.2187(6) 0.5000 0.2471(9) 0.076(3) Uani 1 2 d S
H1W H 0.1970 0.4751 0.2848 0.091 Uiso 1 1 d R
C1 C 0.9811(11) 0.5000 0.3833(13) 0.086(4) Uani 1 2 d SU
H1 H 0.9705 0.5000 0.3018 0.103 Uiso 1 2 calc SR
C2 C 0.8856(8) 0.5000 0.4146(8) 0.038(2) Uani 1 2 d S
C3 C 0.9029(11) 0.5000 0.5329(14) 0.093(5) Uani 1 2 d SU
H3 H 0.8371 0.5000 0.5583 0.112 Uiso 1 2 calc SR
C4 C 0.7634(7) 0.5000 0.3324(9) 0.033(2) Uani 1 2 d S
C5 C 0.3243(7) 0.2716(3) -0.0523(8) 0.060(2) Uani 1 1 d U
H5 H 0.3768 0.2860 -0.0874 0.072 Uiso 1 1 calc R
C6 C 0.2865(6) 0.3044(3) 0.0183(7) 0.0494(19) Uani 1 1 d .
C7 C 0.2109(8) 0.2810(3) 0.0741(11) 0.086(4) Uani 1 1 d .
H7 H 0.1854 0.3023 0.1260 0.103 Uiso 1 1 calc R
C8 C 0.3218(6) 0.3611(3) 0.0433(6) 0.0400(16) Uani 1 1 d .
C9 C 0.5000 0.4682(3) 0.5000 0.034(2) Uani 1 2 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 '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
N2 Fe1 N2 180.000(1) 5_665 .
N2 Fe1 N6 90.51(17) 5_665 5_665
N2 Fe1 N6 89.49(17) . 5_665
N2 Fe1 N6 89.49(17) 5_665 6_565
N2 Fe1 N6 90.51(17) . 6_565
N6 Fe1 N6 87.5(2) 5_665 6_565
N2 Fe1 N6 89.49(17) 5_665 .
N2 Fe1 N6 90.51(17) . .
N6 Fe1 N6 180.0(2) 5_665 .
N6 Fe1 N6 92.5(2) 6_565 .
N2 Fe1 N6 90.51(17) 5_665 2_655
N2 Fe1 N6 89.49(17) . 2_655
N6 Fe1 N6 92.5(2) 5_665 2_655
N6 Fe1 N6 180.00(17) 6_565 2_655
N6 Fe1 N6 87.5(2) . 2_655
O1W Fe2 O1 92.9(2) . 6_565
O1W Fe2 O1 92.9(2) . .
O1 Fe2 O1 79.1(2) 6_565 .
O1W Fe2 N7 91.6(2) . 6_565
O1 Fe2 N7 94.71(18) 6_565 6_565
O1 Fe2 N7 172.51(19) . 6_565
O1W Fe2 N7 91.6(2) . .
O1 Fe2 N7 172.51(19) 6_565 .
O1 Fe2 N7 94.71(18) . .
N7 Fe2 N7 91.1(3) 6_565 .
O1W Fe2 N3 179.2(3) . .
O1 Fe2 N3 87.65(19) 6_565 .
O1 Fe2 N3 87.65(19) . .
N7 Fe2 N3 87.9(2) 6_565 .
N7 Fe2 N3 87.9(2) . .
N2 N1 C4 102.9(7) . .
N2 N1 H1N 128.2 . .
C4 N1 H1N 128.8 . .
N3 N2 N1 110.1(7) . .
N3 N2 Fe1 125.0(5) . .
N1 N2 Fe1 124.9(6) . .
N2 N3 N4 110.8(6) . .
N2 N3 Fe2 125.7(5) . .
N4 N3 Fe2 123.5(5) . .
C4 N4 N3 105.1(7) . .
C4 N4 H4N 128.6 . .
N3 N4 H4N 126.3 . .
C8 N5 N6 104.8(5) . .
C8 N5 H5N 127.6 . .
N6 N5 H5N 127.6 . .
N7 N6 N5 108.3(5) . .
N7 N6 Fe1 125.6(3) . .
N5 N6 Fe1 125.6(4) . .
N6 N7 N8 111.5(5) . .
N6 N7 Fe2 124.7(4) . .
N8 N7 Fe2 123.0(4) . .
N7 N8 C8 104.2(6) . .
N7 N8 H8N 128.5 . .
C8 N8 H8N 127.2 . .
C9 O1 Fe2 112.4(4) . .
Fe2 O1W H1W 117.8 . .
C2 C1 C3 122.4(13) . 5_766
C2 C1 H1 118.8 . .
C3 C1 H1 118.8 5_766 .
C1 C2 C3 117.8(11) . .
C1 C2 C4 125.1(10) . .
C3 C2 C4 117.1(9) . .
C2 C3 C1 119.8(12) . 5_766
C2 C3 H3 120.1 . .
C1 C3 H3 120.1 5_766 .
N4 C4 N1 111.0(7) . .
N4 C4 C2 124.4(8) . .
N1 C4 C2 124.6(8) . .
C7 C5 C6 122.2(8) 7 .
C7 C5 H5 118.9 7 .
C6 C5 H5 118.9 . .
C5 C6 C7 117.9(7) . .
C5 C6 C8 123.9(7) . .
C7 C6 C8 118.2(7) . .
C5 C7 C6 119.9(8) 7 .
C5 C7 H7 120.1 7 .
C6 C7 H7 120.1 . .
N5 C8 N8 111.1(6) . .
N5 C8 C6 123.3(6) . .
N8 C8 C6 125.4(7) . .
O1 C9 O1 125.1(8) . 2_656
O1 C9 C9 117.5(4) . 5_666
O1 C9 C9 117.5(4) 2_656 5_666
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N2 2.083(7) 5_665
Fe1 N2 2.083(7) .
Fe1 N6 2.095(5) 5_665
Fe1 N6 2.095(5) 6_565
Fe1 N6 2.095(5) .
Fe1 N6 2.095(5) 2_655
Fe2 O1W 2.106(7) .
Fe2 O1 2.143(4) 6_565
Fe2 O1 2.143(4) .
Fe2 N7 2.146(5) 6_565
Fe2 N7 2.146(5) .
Fe2 N3 2.180(7) .
N1 N2 1.340(9) .
N1 C4 1.371(12) .
N1 H1N 0.9184 .
N2 N3 1.283(9) .
N3 N4 1.322(10) .
N4 C4 1.314(11) .
N4 H4N 0.9167 .
N5 C8 1.342(9) .
N5 N6 1.352(7) .
N5 H5N 0.8800 .
N6 N7 1.309(7) .
N7 N8 1.322(7) .
N8 C8 1.349(9) .
N8 H8N 0.9177 .
O1 C9 1.262(5) .
O1W H1W 0.8593 .
C1 C2 1.337(15) .
C1 C3 1.413(19) 5_766
C1 H1 0.9500 .
C2 C3 1.374(17) .
C2 C4 1.463(13) .
C3 C1 1.413(19) 5_766
C3 H3 0.9500 .
C5 C7 1.360(10) 7
C5 C6 1.367(10) .
C5 H5 0.9500 .
C6 C7 1.436(10) .
C6 C8 1.461(9) .
C7 C5 1.360(10) 7
C7 H7 0.9500 .
C9 O1 1.262(5) 2_656
C9 C9 1.565(17) 5_666
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 0.0 . .
C4 N1 N2 Fe1 180.000(1) . .
N2 Fe1 N2 N3 -50(100) 5_665 .
N6 Fe1 N2 N3 133.76(12) 5_665 .
N6 Fe1 N2 N3 46.24(12) 6_565 .
N6 Fe1 N2 N3 -46.24(12) . .
N6 Fe1 N2 N3 -133.76(12) 2_655 .
N2 Fe1 N2 N1 130(100) 5_665 .
N6 Fe1 N2 N1 -46.24(12) 5_665 .
N6 Fe1 N2 N1 -133.76(12) 6_565 .
N6 Fe1 N2 N1 133.76(12) . .
N6 Fe1 N2 N1 46.24(12) 2_655 .
N1 N2 N3 N4 0.0 . .
Fe1 N2 N3 N4 180.000(1) . .
N1 N2 N3 Fe2 180.0 . .
Fe1 N2 N3 Fe2 0.0 . .
O1W Fe2 N3 N2 0.00(2) . .
O1 Fe2 N3 N2 -140.42(10) 6_565 .
O1 Fe2 N3 N2 140.42(10) . .
N7 Fe2 N3 N2 -45.61(15) 6_565 .
N7 Fe2 N3 N2 45.61(15) . .
O1W Fe2 N3 N4 180.00(2) . .
O1 Fe2 N3 N4 39.58(10) 6_565 .
O1 Fe2 N3 N4 -39.58(10) . .
N7 Fe2 N3 N4 134.39(15) 6_565 .
N7 Fe2 N3 N4 -134.39(15) . .
N2 N3 N4 C4 0.0 . .
Fe2 N3 N4 C4 180.000(1) . .
C8 N5 N6 N7 -1.9(6) . .
C8 N5 N6 Fe1 170.4(4) . .
N2 Fe1 N6 N7 -133.4(4) 5_665 .
N2 Fe1 N6 N7 46.6(4) . .
N6 Fe1 N6 N7 50(52) 5_665 .
N6 Fe1 N6 N7 -44.0(5) 6_565 .
N6 Fe1 N6 N7 136.0(5) 2_655 .
N2 Fe1 N6 N5 55.6(4) 5_665 .
N2 Fe1 N6 N5 -124.4(4) . .
N6 Fe1 N6 N5 -121(55) 5_665 .
N6 Fe1 N6 N5 145.0(4) 6_565 .
N6 Fe1 N6 N5 -35.0(4) 2_655 .
N5 N6 N7 N8 2.7(7) . .
Fe1 N6 N7 N8 -169.6(4) . .
N5 N6 N7 Fe2 172.6(4) . .
Fe1 N6 N7 Fe2 0.3(6) . .
O1W Fe2 N7 N6 134.5(5) . .
O1 Fe2 N7 N6 -98.6(15) 6_565 .
O1 Fe2 N7 N6 -132.4(5) . .
N7 Fe2 N7 N6 42.9(5) 6_565 .
N3 Fe2 N7 N6 -45.0(5) . .
O1W Fe2 N7 N8 -56.8(5) . .
O1 Fe2 N7 N8 70.1(16) 6_565 .
O1 Fe2 N7 N8 36.2(5) . .
N7 Fe2 N7 N8 -148.4(4) 6_565 .
N3 Fe2 N7 N8 123.7(5) . .
N6 N7 N8 C8 -2.3(7) . .
Fe2 N7 N8 C8 -172.3(4) . .
O1W Fe2 O1 C9 -101.5(3) . .
O1 Fe2 O1 C9 -9.1(3) 6_565 .
N7 Fe2 O1 C9 25.3(16) 6_565 .
N7 Fe2 O1 C9 166.7(3) . .
N3 Fe2 O1 C9 79.0(3) . .
C3 C1 C2 C3 0.000(4) 5_766 .
C3 C1 C2 C4 180.000(3) 5_766 .
C1 C2 C3 C1 0.000(3) . 5_766
C4 C2 C3 C1 180.000(2) . 5_766
N3 N4 C4 N1 0.000(1) . .
N3 N4 C4 C2 180.000(2) . .
N2 N1 C4 N4 0.000(1) . .
N2 N1 C4 C2 180.000(2) . .
C1 C2 C4 N4 180.000(2) . .
C3 C2 C4 N4 0.000(2) . .
C1 C2 C4 N1 0.000(2) . .
C3 C2 C4 N1 180.000(2) . .
C7 C5 C6 C7 2.5(17) 7 .
C7 C5 C6 C8 -179.7(9) 7 .
C5 C6 C7 C5 -2.4(16) . 7
C8 C6 C7 C5 179.7(8) . 7
N6 N5 C8 N8 0.5(7) . .
N6 N5 C8 C6 -175.9(6) . .
N7 N8 C8 N5 1.1(8) . .
N7 N8 C8 C6 177.4(7) . .
C5 C6 C8 N5 15.8(13) . .
C7 C6 C8 N5 -166.3(8) . .
C5 C6 C8 N8 -160.1(8) . .
C7 C6 C8 N8 17.7(12) . .
Fe2 O1 C9 O1 -172.1(3) . 2_656
Fe2 O1 C9 C9 7.9(3) . 5_666
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.014 0.467 -0.003 1904 740 ' '
