#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:38:42 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179590 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/55/4505564.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_4505564
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            'C35 H74 Fe3 N24 O25'
_chemical_formula_weight         1398.73
_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                 110.48(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.078(2)
_cell_length_b                   24.560(5)
_cell_length_c                   12.087(2)
_cell_measurement_temperature    110(2)
_cell_volume                     3358.8(11)
_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 0.963
_diffrn_measured_fraction_theta_max 0.963
_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  0.1015
_diffrn_reflns_av_sigmaI/netI    0.1359
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4437
_diffrn_reflns_theta_full        60.94
_diffrn_reflns_theta_max         60.94
_diffrn_reflns_theta_min         3.60
_exptl_absorpt_coefficient_mu    5.891
_exptl_absorpt_correction_T_max  0.9273
_exptl_absorpt_correction_T_min  0.6192
_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            yellow
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
;
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.870
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         2540
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.870
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0666
_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)+(0.0323P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1400
_refine_ls_wR_factor_ref         0.1508
_reflns_number_gt                1527
_reflns_number_total             2540
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg201569m_si_001.cif
_cod_data_source_block           2.9MeOH(110K)
_cod_original_cell_volume        3359.1(11)
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               4505564
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 0.0412(4) Uani 1 4 d S
Fe2 Fe 0.39561(9) 0.5000 0.25846(11) 0.0465(3) Uani 1 2 d S
N1 N 0.7327(5) 0.5000 0.2151(6) 0.0540(17) Uani 1 2 d S
H1N H 0.7789 0.5000 0.1707 0.065 Uiso 0.17 2 d SPR
N2 N 0.6139(5) 0.5000 0.1746(6) 0.0524(16) Uani 1 2 d S
N3 N 0.5796(5) 0.5000 0.2647(6) 0.0464(15) Uani 1 2 d S
N4 N 0.6687(5) 0.5000 0.3628(6) 0.0534(16) Uani 1 2 d S
H4N H 0.6662 0.5000 0.4364 0.064 Uiso 0.17 2 d SPR
N5 N 0.3715(4) 0.39094(19) -0.0207(4) 0.0591(13) Uani 1 1 d .
H5N H 0.3840 0.3813 -0.0855 0.071 Uiso 0.17 1 calc PR
N6 N 0.3981(3) 0.43856(17) 0.0370(4) 0.0480(11) Uani 1 1 d .
N7 N 0.3639(4) 0.43776(18) 0.1262(4) 0.0500(11) Uani 1 1 d .
N8 N 0.3139(4) 0.38990(18) 0.1326(5) 0.0666(14) Uani 1 1 d .
H8N H 0.2821 0.3793 0.1862 0.080 Uiso 0.17 1 d PR
O1 O 0.4482(3) 0.44532(14) 0.4021(3) 0.0529(9) Uani 1 1 d .
O1W O 0.2110(4) 0.5000 0.2371(6) 0.082(2) Uani 1 2 d S
H1W H 0.1893 0.4751 0.2748 0.098 Uiso 1 1 d R
C1 C 0.9826(7) 0.5000 0.3744(8) 0.090(4) Uani 1 2 d S
H1 H 0.9717 0.5000 0.2926 0.108 Uiso 1 2 calc SR
C2 C 0.8836(6) 0.5000 0.4172(8) 0.058(2) Uani 1 2 d S
C3 C 0.9034(7) 0.5000 0.5362(9) 0.086(3) Uani 1 2 d S
H3 H 0.8366 0.5000 0.5604 0.103 Uiso 1 2 calc SR
C4 C 0.7642(7) 0.5000 0.3322(7) 0.0510(19) Uani 1 2 d S
C5 C 0.3283(5) 0.2711(3) -0.0482(6) 0.0721(19) Uani 1 1 d .
H5 H 0.3832 0.2854 -0.0809 0.087 Uiso 1 1 calc R
C6 C 0.2826(5) 0.3050(3) 0.0193(6) 0.0669(17) Uani 1 1 d .
C7 C 0.2048(5) 0.2814(3) 0.0670(7) 0.082(2) Uani 1 1 d .
H7 H 0.1739 0.3030 0.1146 0.098 Uiso 1 1 calc R
C8 C 0.3220(5) 0.3614(3) 0.0423(6) 0.0632(16) Uani 1 1 d .
C9 C 0.5000 0.4694(3) 0.5000 0.0483(18) 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 90.73(17) 5_665 5_665
N2 Fe1 N6 89.27(17) . 5_665
N2 Fe1 N6 89.27(17) 5_665 .
N2 Fe1 N6 90.73(17) . .
N6 Fe1 N6 180.0(3) 5_665 .
N2 Fe1 N6 90.73(17) 5_665 2_655
N2 Fe1 N6 89.27(17) . 2_655
N6 Fe1 N6 92.3(2) 5_665 2_655
N6 Fe1 N6 87.7(2) . 2_655
N2 Fe1 N6 89.27(17) 5_665 6_565
N2 Fe1 N6 90.73(17) . 6_565
N6 Fe1 N6 87.7(2) 5_665 6_565
N6 Fe1 N6 92.3(2) . 6_565
N6 Fe1 N6 180.0(3) 2_655 6_565
O1 Fe2 O1 79.1(2) 6_565 .
O1 Fe2 N7 94.79(16) 6_565 6_565
O1 Fe2 N7 171.86(16) . 6_565
O1 Fe2 N7 171.86(16) 6_565 .
O1 Fe2 N7 94.79(16) . .
N7 Fe2 N7 90.8(2) 6_565 .
O1 Fe2 O1W 95.73(18) 6_565 .
O1 Fe2 O1W 95.73(18) . .
N7 Fe2 O1W 90.18(17) 6_565 .
N7 Fe2 O1W 90.18(17) . .
O1 Fe2 N3 87.80(17) 6_565 .
O1 Fe2 N3 87.80(17) . .
N7 Fe2 N3 86.60(17) 6_565 .
N7 Fe2 N3 86.60(17) . .
O1W Fe2 N3 175.4(3) . .
C4 N1 N2 105.1(6) . .
C4 N1 H1N 128.9 . .
N2 N1 H1N 126.0 . .
N3 N2 N1 108.0(6) . .
N3 N2 Fe1 124.2(4) . .
N1 N2 Fe1 127.8(6) . .
N4 N3 N2 111.3(6) . .
N4 N3 Fe2 122.7(5) . .
N2 N3 Fe2 126.1(5) . .
N3 N4 C4 105.7(7) . .
N3 N4 H4N 126.9 . .
C4 N4 H4N 127.4 . .
C8 N5 N6 104.5(5) . .
C8 N5 H5N 127.7 . .
N6 N5 H5N 127.7 . .
N7 N6 N5 109.5(4) . .
N7 N6 Fe1 125.3(3) . .
N5 N6 Fe1 124.7(4) . .
N6 N7 N8 110.3(4) . .
N6 N7 Fe2 126.1(3) . .
N8 N7 Fe2 123.4(4) . .
C8 N8 N7 104.5(5) . .
C8 N8 H8N 127.7 . .
N7 N8 H8N 127.8 . .
C9 O1 Fe2 112.2(4) . .
Fe2 O1W H1W 115.7 . .
C3 C1 C2 115.2(8) 5_766 .
C3 C1 H1 122.4 5_766 .
C2 C1 H1 122.4 . .
C3 C2 C4 120.6(7) . .
C3 C2 C1 120.4(7) . .
C4 C2 C1 119.0(8) . .
C2 C3 C1 124.4(8) . 5_766
C2 C3 H3 117.8 . .
C1 C3 H3 117.8 5_766 .
N4 C4 N1 110.0(7) . .
N4 C4 C2 123.2(7) . .
N1 C4 C2 126.7(7) . .
C7 C5 C6 120.8(6) 7 .
C7 C5 H5 119.6 7 .
C6 C5 H5 119.6 . .
C7 C6 C5 116.9(6) . .
C7 C6 C8 122.7(6) . .
C5 C6 C8 120.3(6) . .
C5 C7 C6 122.3(6) 7 .
C5 C7 H7 118.8 7 .
C6 C7 H7 118.8 . .
N8 C8 N5 111.0(5) . .
N8 C8 C6 122.9(6) . .
N5 C8 C6 126.0(6) . .
O1 C9 O1 124.6(7) . 2_656
O1 C9 C9 117.7(3) . 5_666
O1 C9 C9 117.7(3) 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 2.077(7) 5_665
Fe1 N2 2.077(7) .
Fe1 N6 2.092(4) 5_665
Fe1 N6 2.092(4) .
Fe1 N6 2.092(4) 2_655
Fe1 N6 2.092(4) 6_565
Fe2 O1 2.109(4) 6_565
Fe2 O1 2.109(4) .
Fe2 N7 2.148(4) 6_565
Fe2 N7 2.148(4) .
Fe2 O1W 2.153(5) .
Fe2 N3 2.197(6) .
N1 C4 1.330(10) .
N1 N2 1.344(8) .
N1 H1N 0.9000 .
N2 N3 1.294(9) .
N3 N4 1.293(8) .
N4 C4 1.329(9) .
N4 H4N 0.9000 .
N5 C8 1.335(8) .
N5 N6 1.342(6) .
N5 H5N 0.8800 .
N6 N7 1.283(6) .
N7 N8 1.336(6) .
N8 C8 1.328(8) .
N8 H8N 0.9000 .
O1 C9 1.274(5) .
O1W H1W 0.8567 .
C1 C3 1.422(12) 5_766
C1 C2 1.460(12) .
C1 H1 0.9500 .
C2 C3 1.374(13) .
C2 C4 1.448(11) .
C3 C1 1.422(12) 5_766
C3 H3 0.9500 .
C5 C7 1.345(8) 7
C5 C6 1.408(8) .
C5 H5 0.9500 .
C6 C7 1.390(9) .
C6 C8 1.459(8) .
C7 C5 1.345(8) 7
C7 H7 0.9500 .
C9 O1 1.274(5) 2_656
C9 C9 1.502(14) 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 180.0 . .
N2 Fe1 N2 N3 -38(100) 5_665 .
N6 Fe1 N2 N3 133.84(11) 5_665 .
N6 Fe1 N2 N3 -46.16(11) . .
N6 Fe1 N2 N3 -133.84(11) 2_655 .
N6 Fe1 N2 N3 46.16(11) 6_565 .
N2 Fe1 N2 N1 142(100) 5_665 .
N6 Fe1 N2 N1 -46.16(11) 5_665 .
N6 Fe1 N2 N1 133.84(11) . .
N6 Fe1 N2 N1 46.16(11) 2_655 .
N6 Fe1 N2 N1 -133.84(11) 6_565 .
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 . .
O1 Fe2 N3 N4 39.58(10) 6_565 .
O1 Fe2 N3 N4 -39.58(10) . .
N7 Fe2 N3 N4 134.51(12) 6_565 .
N7 Fe2 N3 N4 -134.51(12) . .
O1W Fe2 N3 N4 180.000(4) . .
O1 Fe2 N3 N2 -140.42(10) 6_565 .
O1 Fe2 N3 N2 140.42(10) . .
N7 Fe2 N3 N2 -45.49(12) 6_565 .
N7 Fe2 N3 N2 45.49(12) . .
O1W Fe2 N3 N2 0.000(3) . .
N2 N3 N4 C4 0.0 . .
Fe2 N3 N4 C4 180.000(1) . .
C8 N5 N6 N7 -1.6(5) . .
C8 N5 N6 Fe1 170.8(3) . .
N2 Fe1 N6 N7 -134.0(4) 5_665 .
N2 Fe1 N6 N7 46.0(4) . .
N6 Fe1 N6 N7 110(100) 5_665 .
N6 Fe1 N6 N7 135.2(5) 2_655 .
N6 Fe1 N6 N7 -44.8(5) 6_565 .
N2 Fe1 N6 N5 54.8(4) 5_665 .
N2 Fe1 N6 N5 -125.2(4) . .
N6 Fe1 N6 N5 -61(100) 5_665 .
N6 Fe1 N6 N5 -36.0(3) 2_655 .
N6 Fe1 N6 N5 144.0(3) 6_565 .
N5 N6 N7 N8 0.4(5) . .
Fe1 N6 N7 N8 -171.9(3) . .
N5 N6 N7 Fe2 174.6(3) . .
Fe1 N6 N7 Fe2 2.3(6) . .
O1 Fe2 N7 N6 -93.1(12) 6_565 .
O1 Fe2 N7 N6 -134.0(4) . .
N7 Fe2 N7 N6 40.1(5) 6_565 .
O1W Fe2 N7 N6 130.3(4) . .
N3 Fe2 N7 N6 -46.5(4) . .
O1 Fe2 N7 N8 80.4(12) 6_565 .
O1 Fe2 N7 N8 39.6(4) . .
N7 Fe2 N7 N8 -146.4(3) 6_565 .
O1W Fe2 N7 N8 -56.2(4) . .
N3 Fe2 N7 N8 127.1(4) . .
N6 N7 N8 C8 1.0(6) . .
Fe2 N7 N8 C8 -173.5(4) . .
O1 Fe2 O1 C9 -9.4(3) 6_565 .
N7 Fe2 O1 C9 32.2(12) 6_565 .
N7 Fe2 O1 C9 165.2(2) . .
O1W Fe2 O1 C9 -104.1(2) . .
N3 Fe2 O1 C9 78.8(2) . .
C3 C1 C2 C3 0.000(3) 5_766 .
C3 C1 C2 C4 180.000(2) 5_766 .
C4 C2 C3 C1 180.000(2) . 5_766
C1 C2 C3 C1 0.000(2) . 5_766
N3 N4 C4 N1 0.000(1) . .
N3 N4 C4 C2 180.000(1) . .
N2 N1 C4 N4 0.000(1) . .
N2 N1 C4 C2 180.000(1) . .
C3 C2 C4 N4 0.000(2) . .
C1 C2 C4 N4 180.000(1) . .
C3 C2 C4 N1 180.000(2) . .
C1 C2 C4 N1 0.000(1) . .
C7 C5 C6 C7 1.5(11) 7 .
C7 C5 C6 C8 178.0(7) 7 .
C5 C6 C7 C5 -1.5(12) . 7
C8 C6 C7 C5 -178.0(7) . 7
N7 N8 C8 N5 -2.0(6) . .
N7 N8 C8 C6 177.0(5) . .
N6 N5 C8 N8 2.2(6) . .
N6 N5 C8 C6 -176.8(5) . .
C7 C6 C8 N8 18.7(10) . .
C5 C6 C8 N8 -157.7(6) . .
C7 C6 C8 N5 -162.4(6) . .
C5 C6 C8 N5 21.2(10) . .
Fe2 O1 C9 O1 -171.9(2) . 2_656
Fe2 O1 C9 C9 8.1(2) . 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 -0.013 0.470 0.010 1881 679 ' '
