#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:38:42 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179590 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/55/4505565.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_4505565
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                 110.112(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.0115(10)
_cell_length_b                   24.5797(17)
_cell_length_c                   12.1020(9)
_cell_measurement_temperature    150(2)
_cell_volume                     3355.1(5)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_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  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0623
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4437
_diffrn_reflns_theta_full        61.12
_diffrn_reflns_theta_max         61.12
_diffrn_reflns_theta_min         3.60
_exptl_absorpt_coefficient_mu    5.898
_exptl_absorpt_correction_T_max  0.7374
_exptl_absorpt_correction_T_min  0.6159
_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    1.385
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
;
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.917
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         2542
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0398
_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)+(0.0526P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.1021
_reflns_number_gt                1918
_reflns_number_total             2542
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg201569m_si_001.cif
_cod_data_source_block           2.9MeOH(150K)
_cod_original_cell_volume        3355.1(4)
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               4505565
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 0.0221(2) Uani 1 4 d S
Fe2 Fe 0.39336(6) 0.5000 0.25873(5) 0.0256(2) Uani 1 2 d S
N1 N 0.7335(3) 0.5000 0.2127(3) 0.0340(9) Uani 1 2 d S
H1N H 0.7799 0.5000 0.1680 0.041 Uiso 0.17 2 d SPR
N2 N 0.6138(3) 0.5000 0.1737(3) 0.0275(8) Uani 1 2 d S
N3 N 0.5761(3) 0.5000 0.2631(3) 0.0283(8) Uani 1 2 d S
N4 N 0.6685(3) 0.5000 0.3641(3) 0.0347(9) Uani 1 2 d S
H4N H 0.6660 0.5000 0.4376 0.042 Uiso 0.17 2 d SPR
N5 N 0.3696(2) 0.39099(11) -0.0198(2) 0.0400(7) Uani 1 1 d .
H5N H 0.3832 0.3809 -0.0838 0.048 Uiso 0.17 1 calc PR
N6 N 0.3961(2) 0.43858(10) 0.0363(2) 0.0320(6) Uani 1 1 d .
N7 N 0.3607(2) 0.43764(11) 0.1283(2) 0.0368(7) Uani 1 1 d .
N8 N 0.3111(3) 0.38984(11) 0.1351(3) 0.0466(8) Uani 1 1 d .
H8N H 0.2792 0.3792 0.1889 0.056 Uiso 0.17 1 d PR
O1 O 0.44819(18) 0.44516(8) 0.40361(17) 0.0310(5) Uani 1 1 d .
O1W O 0.2136(3) 0.5000 0.2435(4) 0.0743(13) Uani 1 2 d S
H1W H 0.1920 0.4753 0.2809 0.089 Uiso 1 1 d R
C1 C 0.9828(5) 0.5000 0.3823(5) 0.0618(17) Uani 1 2 d SU
H1 H 0.9722 0.5000 0.3009 0.074 Uiso 1 2 calc SR
C2 C 0.8855(4) 0.5000 0.4173(4) 0.0378(11) Uani 1 2 d S
C3 C 0.9021(5) 0.5000 0.5339(5) 0.0633(17) Uani 1 2 d SU
H3 H 0.8354 0.5000 0.5592 0.076 Uiso 1 2 calc SR
C4 C 0.7635(4) 0.5000 0.3306(4) 0.0341(11) Uani 1 2 d S
C5 C 0.3283(4) 0.27245(16) -0.0468(4) 0.0588(11) Uani 1 1 d .
H5 H 0.3825 0.2877 -0.0799 0.071 Uiso 1 1 calc R
C6 C 0.2821(3) 0.30468(15) 0.0193(3) 0.0484(9) Uani 1 1 d .
C7 C 0.2027(4) 0.28201(16) 0.0662(4) 0.0625(12) Uani 1 1 d .
H7 H 0.1693 0.3038 0.1117 0.075 Uiso 1 1 calc R
C8 C 0.3180(3) 0.36209(14) 0.0424(3) 0.0430(9) Uani 1 1 d .
C9 C 0.5000 0.46864(17) 0.5000 0.0270(9) 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 91.13(9) 5_665 5_665
N2 Fe1 N6 88.87(9) . 5_665
N2 Fe1 N6 88.87(9) 5_665 .
N2 Fe1 N6 91.13(9) . .
N6 Fe1 N6 180.00(13) 5_665 .
N2 Fe1 N6 88.87(9) 5_665 6_565
N2 Fe1 N6 91.13(9) . 6_565
N6 Fe1 N6 88.01(14) 5_665 6_565
N6 Fe1 N6 91.99(14) . 6_565
N2 Fe1 N6 91.13(9) 5_665 2_655
N2 Fe1 N6 88.87(9) . 2_655
N6 Fe1 N6 91.99(14) 5_665 2_655
N6 Fe1 N6 88.01(14) . 2_655
N6 Fe1 N6 180.00(10) 6_565 2_655
O1W Fe2 O1 95.16(11) . 6_565
O1W Fe2 O1 95.16(11) . .
O1 Fe2 O1 78.59(11) 6_565 .
O1W Fe2 N7 90.74(12) . 6_565
O1 Fe2 N7 94.60(9) 6_565 6_565
O1 Fe2 N7 171.34(10) . 6_565
O1W Fe2 N7 90.74(12) . .
O1 Fe2 N7 171.34(10) 6_565 .
O1 Fe2 N7 94.60(9) . .
N7 Fe2 N7 91.64(15) 6_565 .
O1W Fe2 N3 176.59(16) . .
O1 Fe2 N3 87.48(9) 6_565 .
O1 Fe2 N3 87.48(9) . .
N7 Fe2 N3 86.88(10) 6_565 .
N7 Fe2 N3 86.88(10) . .
C4 N1 N2 103.6(3) . .
C4 N1 H1N 129.8 . .
N2 N1 H1N 126.6 . .
N3 N2 N1 109.9(3) . .
N3 N2 Fe1 122.9(2) . .
N1 N2 Fe1 127.2(3) . .
N2 N3 N4 110.0(3) . .
N2 N3 Fe2 127.7(2) . .
N4 N3 Fe2 122.3(3) . .
C4 N4 N3 104.4(3) . .
C4 N4 H4N 128.5 . .
N3 N4 H4N 127.1 . .
C8 N5 N6 104.8(3) . .
C8 N5 H5N 127.6 . .
N6 N5 H5N 127.6 . .
N7 N6 N5 108.9(3) . .
N7 N6 Fe1 125.14(19) . .
N5 N6 Fe1 125.4(2) . .
N6 N7 N8 110.3(2) . .
N6 N7 Fe2 125.4(2) . .
N8 N7 Fe2 124.0(2) . .
N7 N8 C8 103.8(3) . .
N7 N8 H8N 127.7 . .
C8 N8 H8N 128.4 . .
C9 O1 Fe2 112.8(2) . .
Fe2 O1W H1W 116.4 . .
C2 C1 C3 120.6(5) . 5_766
C2 C1 H1 119.7 . .
C3 C1 H1 119.7 5_766 .
C3 C2 C1 119.0(5) . .
C3 C2 C4 119.5(4) . .
C1 C2 C4 121.5(4) . .
C2 C3 C1 120.4(5) . 5_766
C2 C3 H3 119.8 . .
C1 C3 H3 119.8 5_766 .
N4 C4 N1 112.1(4) . .
N4 C4 C2 121.7(4) . .
N1 C4 C2 126.2(4) . .
C6 C5 C7 121.1(4) . 7
C6 C5 H5 119.4 . .
C7 C5 H5 119.4 7 .
C5 C6 C7 118.7(3) . .
C5 C6 C8 120.9(4) . .
C7 C6 C8 120.3(3) . .
C6 C7 C5 120.1(4) . 7
C6 C7 H7 119.9 . .
C5 C7 H7 119.9 7 .
N5 C8 N8 112.1(3) . .
N5 C8 C6 124.4(3) . .
N8 C8 C6 123.2(3) . .
O1 C9 O1 125.4(4) . 2_656
O1 C9 C9 117.32(19) . 5_666
O1 C9 C9 117.32(19) 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 2.076(3) 5_665
Fe1 N2 2.076(3) .
Fe1 N6 2.099(3) 5_665
Fe1 N6 2.099(3) .
Fe1 N6 2.099(3) 6_565
Fe1 N6 2.099(3) 2_655
Fe2 O1W 2.103(3) .
Fe2 O1 2.129(2) 6_565
Fe2 O1 2.129(2) .
Fe2 N7 2.137(3) 6_565
Fe2 N7 2.137(3) .
Fe2 N3 2.177(3) .
N1 C4 1.347(6) .
N1 N2 1.350(5) .
N1 H1N 0.9000 .
N2 N3 1.309(5) .
N3 N4 1.339(5) .
N4 C4 1.336(6) .
N4 H4N 0.8999 .
N5 C8 1.333(4) .
N5 N6 1.335(4) .
N5 H5N 0.8800 .
N6 N7 1.322(4) .
N7 N8 1.333(4) .
N8 C8 1.340(4) .
N8 H8N 0.9001 .
O1 C9 1.258(3) .
O1W H1W 0.8499 .
C1 C2 1.373(7) .
C1 C3 1.406(8) 5_766
C1 H1 0.9500 .
C2 C3 1.356(7) .
C2 C4 1.480(6) .
C3 C1 1.406(8) 5_766
C3 H3 0.9500 .
C5 C6 1.371(5) .
C5 C7 1.388(5) 7
C5 H5 0.9500 .
C6 C7 1.384(5) .
C6 C8 1.474(5) .
C7 C5 1.388(5) 7
C7 H7 0.9500 .
C9 O1 1.258(3) 2_656
C9 C9 1.541(8) 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 -67(23) 5_665 .
N6 Fe1 N2 N3 133.99(7) 5_665 .
N6 Fe1 N2 N3 -46.01(7) . .
N6 Fe1 N2 N3 46.01(7) 6_565 .
N6 Fe1 N2 N3 -133.99(7) 2_655 .
N2 Fe1 N2 N1 113(100) 5_665 .
N6 Fe1 N2 N1 -46.01(7) 5_665 .
N6 Fe1 N2 N1 133.99(7) . .
N6 Fe1 N2 N1 -133.99(7) 6_565 .
N6 Fe1 N2 N1 46.01(7) 2_655 .
N1 N2 N3 N4 0.0 . .
Fe1 N2 N3 N4 180.0 . .
N1 N2 N3 Fe2 180.0 . .
Fe1 N2 N3 Fe2 0.0 . .
O1W Fe2 N3 N2 0.000(3) . .
O1 Fe2 N3 N2 -140.66(5) 6_565 .
O1 Fe2 N3 N2 140.66(5) . .
N7 Fe2 N3 N2 -45.91(7) 6_565 .
N7 Fe2 N3 N2 45.91(7) . .
O1W Fe2 N3 N4 180.000(3) . .
O1 Fe2 N3 N4 39.34(5) 6_565 .
O1 Fe2 N3 N4 -39.34(5) . .
N7 Fe2 N3 N4 134.09(7) 6_565 .
N7 Fe2 N3 N4 -134.09(7) . .
N2 N3 N4 C4 0.0 . .
Fe2 N3 N4 C4 180.0 . .
C8 N5 N6 N7 -0.2(3) . .
C8 N5 N6 Fe1 171.1(2) . .
N2 Fe1 N6 N7 -134.6(2) 5_665 .
N2 Fe1 N6 N7 45.4(2) . .
N6 Fe1 N6 N7 110(14) 5_665 .
N6 Fe1 N6 N7 -45.7(3) 6_565 .
N6 Fe1 N6 N7 134.3(3) 2_655 .
N2 Fe1 N6 N5 55.4(2) 5_665 .
N2 Fe1 N6 N5 -124.6(2) . .
N6 Fe1 N6 N5 -60(14) 5_665 .
N6 Fe1 N6 N5 144.3(2) 6_565 .
N6 Fe1 N6 N5 -35.7(2) 2_655 .
N5 N6 N7 N8 0.3(3) . .
Fe1 N6 N7 N8 -171.1(2) . .
N5 N6 N7 Fe2 174.4(2) . .
Fe1 N6 N7 Fe2 3.0(3) . .
O1W Fe2 N7 N6 131.2(3) . .
O1 Fe2 N7 N6 -95.8(7) 6_565 .
O1 Fe2 N7 N6 -133.6(2) . .
N7 Fe2 N7 N6 40.4(3) 6_565 .
N3 Fe2 N7 N6 -46.4(2) . .
O1W Fe2 N7 N8 -55.5(3) . .
O1 Fe2 N7 N8 77.5(7) 6_565 .
O1 Fe2 N7 N8 39.7(3) . .
N7 Fe2 N7 N8 -146.3(2) 6_565 .
N3 Fe2 N7 N8 126.9(3) . .
N6 N7 N8 C8 -0.2(4) . .
Fe2 N7 N8 C8 -174.4(2) . .
O1W Fe2 O1 C9 -103.37(15) . .
O1 Fe2 O1 C9 -9.13(17) 6_565 .
N7 Fe2 O1 C9 29.4(7) 6_565 .
N7 Fe2 O1 C9 165.47(14) . .
N3 Fe2 O1 C9 78.80(14) . .
C3 C1 C2 C3 0.000(1) 5_766 .
C3 C1 C2 C4 180.0 5_766 .
C1 C2 C3 C1 0.000(1) . 5_766
C4 C2 C3 C1 180.000(1) . 5_766
N3 N4 C4 N1 0.0 . .
N3 N4 C4 C2 180.0 . .
N2 N1 C4 N4 0.0 . .
N2 N1 C4 C2 180.0 . .
C3 C2 C4 N4 0.0 . .
C1 C2 C4 N4 180.0 . .
C3 C2 C4 N1 180.000(1) . .
C1 C2 C4 N1 0.000(1) . .
C7 C5 C6 C7 -0.5(7) 7 .
C7 C5 C6 C8 178.2(4) 7 .
C5 C6 C7 C5 0.5(7) . 7
C8 C6 C7 C5 -178.2(4) . 7
N6 N5 C8 N8 0.1(4) . .
N6 N5 C8 C6 -174.7(3) . .
N7 N8 C8 N5 0.1(4) . .
N7 N8 C8 C6 174.9(3) . .
C5 C6 C8 N5 18.3(6) . .
C7 C6 C8 N5 -163.0(4) . .
C5 C6 C8 N8 -155.9(4) . .
C7 C6 C8 N8 22.8(6) . .
Fe2 O1 C9 O1 -172.06(15) . 2_656
Fe2 O1 C9 C9 7.94(15) . 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 0.469 0.006 1882 543 ' '
