#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/55/4505560.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_4505560
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            'C12 H20 Fe N12 O6.5'
_chemical_formula_weight         492.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           166
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   22.505(3)
_cell_length_b                   22.505(3)
_cell_length_c                   7.3716(19)
_cell_measurement_temperature    100(2)
_cell_volume                     3233.3(10)
_computing_cell_refinement       'Bruker SMART (Bruker, 1998)'
_computing_data_collection       'Bruker SMART (Bruker, 1998)'
_computing_data_reduction        'Bruker SAINT + & SHELXTL (Bruker, 1998)'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0277
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       2
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2918
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.758
_exptl_absorpt_correction_T_max  0.9703
_exptl_absorpt_correction_T_min  0.9349
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1524
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
;
_refine_diff_density_max         0.796
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.0010(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     69
_refine_ls_number_reflns         753
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0523
_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)+(0.0850P)²+12.8210P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1433
_refine_ls_wR_factor_ref         0.1473
_reflns_number_gt                673
_reflns_number_total             753
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg201569m_si_001.cif
_cod_data_source_block           1.13H2O(100K)
_cod_original_cell_volume        3233.4(10)
_cod_original_sg_symbol_H-M      R-3m
_cod_original_formula_sum        'C12 H20 Fe N12 O6.50'
_cod_database_code               4505560
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
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 0.0000 0.0000 0.0000 0.0125(4) Uani 1 12 d S
Fe2 Fe 0.0000 0.0000 0.5000 0.0121(4) Uani 1 12 d S
N1 N 0.07642(10) 0.1528(2) 0.1241(5) 0.0405(11) Uani 1 2 d S
H1N H 0.0851 0.1703 0.0123 0.049 Uiso 0.17 2 d SPR
N2 N 0.04337(9) 0.08675(18) 0.1716(4) 0.0248(9) Uani 1 2 d S
N3 N 0.04135(8) 0.08270(17) 0.3513(4) 0.0183(7) Uani 1 2 d S
N4 N 0.07256(9) 0.14513(17) 0.4240(4) 0.0246(8) Uani 1 2 d S
H4N H 0.0781 0.1561 0.5413 0.030 Uiso 0.17 2 d SPR
C1 C 0.1495(5) 0.3612(4) 0.4788(10) 0.064(3) Uani 0.50 1 d P
H1 H 0.1374 0.3802 0.5776 0.077 Uiso 0.50 1 d PR
C2 C 0.1150(5) 0.2904(4) 0.4485(11) 0.061(3) Uani 0.50 1 d P
H2 H 0.0794 0.2614 0.5300 0.073 Uiso 0.50 1 d PR
C3 C 0.13135(12) 0.2627(2) 0.3051(7) 0.0510(16) Uani 1 2 d S
C4 C 0.09406(12) 0.1881(2) 0.2807(6) 0.0359(12) Uani 1 2 d S
O1W O 0.1279(4) 0.2086(3) -0.2238(7) 0.074(3) Uani 0.50 1 d PU
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'
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
N2 Fe1 N2 180.0(2) 19 .
N2 Fe1 N2 87.81(13) 19 20
N2 Fe1 N2 92.19(13) . 20
N2 Fe1 N2 87.81(13) 19 21
N2 Fe1 N2 92.19(13) . 21
N2 Fe1 N2 87.81(13) 20 21
N2 Fe1 N2 92.19(13) 19 3
N2 Fe1 N2 87.81(13) . 3
N2 Fe1 N2 92.19(13) 20 3
N2 Fe1 N2 180.00(16) 21 3
N2 Fe1 N2 92.19(13) 19 2
N2 Fe1 N2 87.81(13) . 2
N2 Fe1 N2 180.00(16) 20 2
N2 Fe1 N2 92.19(13) 21 2
N2 Fe1 N2 87.81(13) 3 2
N3 Fe2 N3 88.54(13) 21_556 2
N3 Fe2 N3 91.46(13) 21_556 20_556
N3 Fe2 N3 180.00(15) 2 20_556
N3 Fe2 N3 180.00(8) 21_556 3
N3 Fe2 N3 91.46(13) 2 3
N3 Fe2 N3 88.54(13) 20_556 3
N3 Fe2 N3 88.54(13) 21_556 .
N3 Fe2 N3 91.46(13) 2 .
N3 Fe2 N3 88.54(13) 20_556 .
N3 Fe2 N3 91.46(13) 3 .
N3 Fe2 N3 91.46(13) 21_556 19_556
N3 Fe2 N3 88.54(13) 2 19_556
N3 Fe2 N3 91.46(13) 20_556 19_556
N3 Fe2 N3 88.54(13) 3 19_556
N3 Fe2 N3 180.00(15) . 19_556
N2 N1 C4 105.6(3) . .
N2 N1 H1N 127.6 . .
C4 N1 H1N 126.8 . .
N3 N2 N1 108.6(3) . .
N3 N2 Fe1 123.4(3) . .
N1 N2 Fe1 128.0(3) . .
N2 N3 N4 110.4(3) . .
N2 N3 Fe2 127.6(3) . .
N4 N3 Fe2 122.0(2) . .
N3 N4 C4 104.7(3) . .
N3 N4 H4N 127.7 . .
C4 N4 H4N 127.7 . .
C3 C1 C2 119.1(7) 31 .
C3 C1 C1 59.8(4) 31 23
C2 C1 C1 89.3(6) . 23
C3 C1 C2 44.8(4) 31 17
C2 C1 C2 89.5(5) . 17
C1 C1 C2 89.5(4) 23 17
C3 C1 C2 89.8(6) 31 23
C2 C1 C2 43.9(7) . 23
C1 C1 C2 45.3(4) 23 23
C2 C1 C2 89.2(5) 17 23
C3 C1 H1 120.0 31 .
C2 C1 H1 120.9 . .
C1 C1 H1 120.8 23 .
C2 C1 H1 134.6 17 .
C2 C1 H1 136.1 23 .
C2 C2 C3 60.2(5) 23 .
C2 C2 C1 90.7(6) 23 .
C3 C2 C1 121.3(7) . .
C2 C2 C1 90.5(4) 23 17
C3 C2 C1 45.6(4) . 17
C1 C2 C1 90.5(5) . 17
C2 C2 C1 45.3(4) 23 23
C3 C2 C1 90.9(6) . 23
C1 C2 C1 45.4(7) . 23
C1 C2 C1 90.8(5) 17 23
C2 C2 H2 119.8 23 .
C3 C2 H2 120.0 . .
C1 C2 H2 118.7 . .
C1 C2 H2 135.1 17 .
C1 C2 H2 134.1 23 .
C2 C3 C2 59.7(9) 23 .
C2 C3 C1 119.6(6) 23 17
C2 C3 C1 89.6(5) . 17
C2 C3 C1 89.6(5) 23 31
C2 C3 C1 119.6(6) . 31
C1 C3 C1 60.4(8) 17 31
C2 C3 C4 119.1(4) 23 .
C2 C3 C4 119.1(4) . .
C1 C3 C4 121.3(5) 17 .
C1 C3 C4 121.3(5) 31 .
N1 C4 N4 110.8(4) . .
N1 C4 C3 127.8(4) . .
N4 C4 C3 121.4(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N2 2.112(3) 19
Fe1 N2 2.112(3) .
Fe1 N2 2.112(3) 20
Fe1 N2 2.112(3) 21
Fe1 N2 2.112(3) 3
Fe1 N2 2.112(3) 2
Fe2 N3 1.949(3) 21_556
Fe2 N3 1.949(3) 2
Fe2 N3 1.949(3) 20_556
Fe2 N3 1.949(3) 3
Fe2 N3 1.949(3) .
Fe2 N3 1.949(3) 19_556
N1 N2 1.335(5) .
N1 C4 1.344(6) .
N1 H1N 0.8915 .
N2 N3 1.327(4) .
N3 N4 1.330(5) .
N4 C4 1.348(5) .
N4 H4N 0.8910 .
C1 C3 1.389(8) 31
C1 C2 1.397(10) .
C1 C1 1.40(2) 23
C1 C2 1.943(10) 17
C1 C2 1.964(13) 23
C1 H1 0.9516 .
C2 C2 1.36(2) 23
C2 C3 1.369(9) .
C2 C1 1.943(10) 17
C2 C1 1.964(13) 23
C2 H2 0.9524 .
C3 C2 1.369(9) 23
C3 C1 1.389(8) 17
C3 C1 1.389(8) 31
C3 C4 1.465(7) .
O1W O1W 1.062(15) 23
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 0.000 0.333 -0.040 83 38 ' '
2 0.000 0.667 -0.040 83 38 ' '
3 0.333 0.000 -0.040 83 38 ' '
4 0.333 0.333 -0.041 83 38 ' '
5 0.667 0.667 -0.040 83 38 ' '
6 0.667 1.000 -0.040 83 38 ' '
