#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/55/4505561.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_4505561
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                   22.6476(11)
_cell_length_b                   22.6476(11)
_cell_length_c                   7.4471(5)
_cell_measurement_temperature    150(2)
_cell_volume                     3308.0(3)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'PROCESS-AUTO (Rigaku, 1998)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IP'
_diffrn_measurement_method       'ω 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  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3140
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         3.44
_exptl_absorpt_coefficient_mu    0.741
_exptl_absorpt_correction_T_max  0.9710
_exptl_absorpt_correction_T_min  0.9363
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.483
_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         1.031
_refine_diff_density_min         -0.910
_refine_diff_density_rms         0.136
_refine_ls_extinction_coef       0.0030(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.206
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     69
_refine_ls_number_reflns         765
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.219
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0528
_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)+(0.0804P)²+30.4581P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.1885
_reflns_number_gt                567
_reflns_number_total             765
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg201569m_si_001.cif
_cod_data_source_block           1.13H2O(150K)
_cod_original_sg_symbol_H-M      R-3m
_cod_original_formula_sum        'C12 H20 Fe N12 O6.50'
_cod_database_code               4505561
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 0.0149(6) Uani 1 12 d S
Fe2 Fe 0.0000 0.0000 0.5000 0.0147(6) Uani 1 12 d S
N1 N 0.07672(13) 0.1534(3) 0.1295(7) 0.0309(14) Uani 1 2 d S
H1N H 0.0854 0.1709 0.0177 0.037 Uiso 0.17 2 d SPR
N2 N 0.04400(13) 0.0880(3) 0.1762(6) 0.0231(12) Uani 1 2 d S
N3 N 0.04150(13) 0.0830(3) 0.3532(6) 0.0196(11) Uani 1 2 d S
N4 N 0.07253(12) 0.1451(2) 0.4264(7) 0.0222(12) Uani 1 2 d S
H4N H 0.0780 0.1560 0.5437 0.027 Uiso 0.17 2 d SPR
C1 C 0.1491(6) 0.3612(5) 0.4748(14) 0.047(3) Uani 0.50 1 d P
H1 H 0.1369 0.3802 0.5736 0.057 Uiso 0.50 1 d PR
C2 C 0.1162(7) 0.2919(6) 0.4500(15) 0.046(3) Uani 0.50 1 d P
H2 H 0.0806 0.2628 0.5315 0.056 Uiso 0.50 1 d PR
C3 C 0.13141(17) 0.2628(3) 0.3081(9) 0.0344(18) Uani 1 2 d S
C4 C 0.09390(16) 0.1878(3) 0.2851(8) 0.0247(15) Uani 1 2 d S
O1W O 0.1279(5) 0.2094(5) -0.2185(10) 0.071(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(3) . 19
N2 Fe1 N2 87.16(19) . 2
N2 Fe1 N2 92.84(19) 19 2
N2 Fe1 N2 87.16(19) . 3
N2 Fe1 N2 92.84(19) 19 3
N2 Fe1 N2 87.16(19) 2 3
N2 Fe1 N2 92.84(19) . 21
N2 Fe1 N2 87.16(19) 19 21
N2 Fe1 N2 92.84(19) 2 21
N2 Fe1 N2 180.0(2) 3 21
N2 Fe1 N2 92.84(19) . 20
N2 Fe1 N2 87.16(19) 19 20
N2 Fe1 N2 180.0(4) 2 20
N2 Fe1 N2 92.84(19) 3 20
N2 Fe1 N2 87.16(19) 21 20
N3 Fe2 N3 180.0(2) 2 20_556
N3 Fe2 N3 88.06(19) 2 21_556
N3 Fe2 N3 91.94(19) 20_556 21_556
N3 Fe2 N3 88.06(19) 2 19_556
N3 Fe2 N3 91.94(19) 20_556 19_556
N3 Fe2 N3 91.94(19) 21_556 19_556
N3 Fe2 N3 91.94(19) 2 3
N3 Fe2 N3 88.06(19) 20_556 3
N3 Fe2 N3 180.00(12) 21_556 3
N3 Fe2 N3 88.06(19) 19_556 3
N3 Fe2 N3 91.94(19) 2 .
N3 Fe2 N3 88.06(19) 20_556 .
N3 Fe2 N3 88.06(19) 21_556 .
N3 Fe2 N3 180.0(2) 19_556 .
N3 Fe2 N3 91.94(19) 3 .
N2 N1 C4 105.0(5) . .
N2 N1 H1N 127.5 . .
C4 N1 H1N 127.5 . .
N3 N2 N1 109.4(5) . .
N3 N2 Fe1 123.0(4) . .
N1 N2 Fe1 127.6(4) . .
N2 N3 N4 109.9(5) . .
N2 N3 Fe2 128.1(4) . .
N4 N3 Fe2 122.0(4) . .
N3 N4 C4 104.4(5) . .
N3 N4 H4N 128.0 . .
C4 N4 H4N 127.6 . .
C2 C1 C3 119.6(10) . 31
C2 C1 C1 88.4(8) . 23
C3 C1 C1 59.3(6) 31 23
C2 C1 C2 90.1(8) . 17
C3 C1 C2 45.2(5) 31 17
C1 C1 C2 88.8(6) 23 17
C2 C1 C2 43.7(9) . 23
C3 C1 C2 89.7(7) 31 23
C1 C1 C2 44.6(5) 23 23
C2 C1 C2 89.3(7) 17 23
C2 C1 H1 120.2 . .
C3 C1 H1 120.2 31 .
C1 C1 H1 120.8 23 .
C2 C1 H1 135.7 17 .
C2 C1 H1 135.0 23 .
C2 C2 C1 91.6(8) 23 .
C2 C2 C3 60.7(6) 23 .
C1 C2 C3 121.9(10) . .
C2 C2 C1 91.1(6) 23 17
C1 C2 C1 89.8(8) . 17
C3 C2 C1 46.1(5) . 17
C2 C2 C1 44.6(5) 23 23
C1 C2 C1 47.0(10) . 23
C3 C2 C1 90.7(8) . 23
C1 C2 C1 90.7(7) 17 23
C2 C2 H2 119.8 23 .
C1 C2 H2 119.3 . .
C3 C2 H2 118.8 . .
C1 C2 H2 134.3 17 .
C1 C2 H2 135.0 23 .
C2 C3 C2 58.7(12) 23 .
C2 C3 C1 118.4(8) 23 17
C2 C3 C1 88.7(7) . 17
C2 C3 C1 88.7(7) 23 31
C2 C3 C1 118.4(8) . 31
C1 C3 C1 61.3(11) 17 31
C2 C3 C4 120.0(7) 23 .
C2 C3 C4 120.0(7) . .
C1 C3 C4 121.5(6) 17 .
C1 C3 C4 121.5(6) 31 .
N1 C4 N4 111.3(5) . .
N1 C4 C3 126.8(6) . .
N4 C4 C3 121.9(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N2 2.168(5) .
Fe1 N2 2.168(5) 19
Fe1 N2 2.168(5) 2
Fe1 N2 2.168(5) 3
Fe1 N2 2.168(5) 21
Fe1 N2 2.168(5) 20
Fe2 N3 1.961(5) 2
Fe2 N3 1.961(5) 20_556
Fe2 N3 1.961(5) 21_556
Fe2 N3 1.961(5) 19_556
Fe2 N3 1.961(5) 3
Fe2 N3 1.961(5) .
N1 N2 1.330(7) .
N1 C4 1.341(8) .
N1 H1N 0.9001 .
N2 N3 1.321(6) .
N3 N4 1.334(7) .
N4 C4 1.345(8) .
N4 H4N 0.8999 .
C1 C2 1.371(15) .
C1 C3 1.400(12) 31
C1 C1 1.43(3) 23
C1 C2 1.941(15) 17
C1 C2 1.951(18) 23
C1 H1 0.9598 .
C2 C2 1.35(3) 23
C2 C3 1.377(12) .
C2 C1 1.941(15) 17
C2 C1 1.951(18) 23
C2 H2 0.9599 .
C3 C2 1.377(12) 23
C3 C1 1.400(12) 17
C3 C1 1.400(12) 31
C3 C4 1.481(9) .
O1W O1W 1.05(2) 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 -0.034 88 24 ' '
2 0.000 0.667 -0.034 88 24 ' '
3 0.333 0.000 -0.034 88 24 ' '
4 0.333 0.333 -0.038 88 23 ' '
5 0.667 0.667 -0.033 88 23 ' '
6 0.667 1.000 -0.032 88 24 ' '
