#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:03:40 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179465 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/62/4336257.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_4336257
loop_
_publ_author_name
'Arpan Hazra'
'Satyanarayana Bonakala'
'Sandeep K. Reddy'
'Sundaram Balasubramanian'
'Tapas Kumar Maji'
_publ_section_title
;
 Effect of Pillar Modules and Their Stoichiometry in 3D Porous Frameworks
 of Zn(II) with [Fe(CN)6]3-: High CO2/N2 and CO2/CH4 Selectivity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11385
_journal_page_last               11397
_journal_paper_doi               10.1021/ic401657d
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C32 H24 Fe2 N20 O6 Zn3'
_chemical_formula_weight         1092.52
_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                 99.799(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   23.1680(17)
_cell_length_b                   7.5344(5)
_cell_length_c                   13.4973(9)
_cell_measurement_reflns_used    5637
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      24.98
_cell_measurement_theta_min      2.10
_cell_volume                     2321.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT  A'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      290(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and 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  0.1423
_diffrn_reflns_av_sigmaI/netI    0.1246
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10514
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.85
_exptl_absorpt_coefficient_mu    2.199
_exptl_absorpt_correction_T_max  0.8613
_exptl_absorpt_correction_T_min  0.7338
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_description       block
_exptl_crystal_F_000             1092
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.934
_refine_diff_density_min         -0.992
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         2203
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1404
_refine_ls_R_factor_gt           0.0640
_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)+(0.0663P)²+1.5806P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1760
_reflns_number_gt                1166
_reflns_number_total             2203
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic401657d_si_002_3.cif
_cod_data_source_block           Compound3
_cod_database_code               4336257
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
C1 C 0.5914(3) 0.8168(11) 0.0864(6) 0.035(2) Uani 1 1 d .
C2 C 0.7075(3) 1.1760(11) 0.1637(5) 0.033(2) Uani 1 1 d .
C3 C 0.6659(5) 1.0000 -0.0115(10) 0.036(3) Uani 1 2 d S
C4 C 0.6233(5) 1.0000 0.2555(8) 0.038(3) Uani 1 2 d S
C5 C 0.4013(6) 0.5000 0.1263(10) 0.072(2) Uani 1 2 d S
H5 H 0.3784 0.5000 0.0626 0.086 Uiso 1 2 calc SR
C6 C 0.4898(6) 0.5000 0.2233(10) 0.072(2) Uani 1 2 d S
H6 H 0.5304 0.5000 0.2303 0.086 Uiso 1 2 calc SR
C7 C 0.3724(6) 0.5000 0.2081(9) 0.072(2) Uani 1 2 d S
H7 H 0.3318 0.5000 0.2004 0.086 Uiso 1 2 calc SR
C8 C 0.4648(6) 0.5000 0.3085(10) 0.072(2) Uani 1 2 d S
H8 H 0.4878 0.5000 0.3721 0.086 Uiso 1 2 calc SR
C9 C 0.4055(6) 0.5000 0.2969(10) 0.072(2) Uani 1 2 d S
C10 C 0.3042(6) 0.5000 0.4694(9) 0.051(4) Uani 1 2 d S
C11 C 0.2452(6) 0.5000 0.4576(10) 0.073(5) Uani 1 2 d S
H11 H 0.2231 0.5000 0.3932 0.088 Uiso 1 2 calc SR
C12 C 0.3358(6) 0.5000 0.5672(9) 0.066(5) Uani 1 2 d S
H12 H 0.3766 0.5000 0.5800 0.079 Uiso 1 2 calc SR
C13 C 0.2179(5) 0.5000 0.5380(9) 0.056(4) Uani 1 2 d S
H13 H 0.1772 0.5000 0.5266 0.068 Uiso 1 2 calc SR
C14 C 0.3036(6) 0.5000 0.6431(9) 0.063(4) Uani 1 2 d S
H14 H 0.3243 0.5000 0.7085 0.075 Uiso 1 2 calc SR
N1 N 0.5590(3) 0.7010(9) 0.0641(5) 0.0392(18) Uani 1 1 d .
N2 N 0.7436(3) 1.2810(9) 0.1876(5) 0.0400(18) Uani 1 1 d .
N3 N 0.6746(4) 1.0000 -0.0918(7) 0.042(3) Uani 1 2 d S
N4 N 0.6054(5) 1.0000 0.3295(9) 0.070(4) Uani 1 2 d S
N5 N 0.4587(4) 0.5000 0.1317(7) 0.039(3) Uani 1 2 d S
N6 N 0.3811(6) 0.5000 0.3937(8) 0.083(4) Uani 1 2 d S
N7 N 0.3308(5) 0.5000 0.3819(8) 0.073(4) Uani 1 2 d S
N8 N 0.2456(4) 0.5000 0.6325(7) 0.044(3) Uani 1 2 d S
O1 O 0.8736(3) 1.5000 0.3022(6) 0.057(3) Uani 1 2 d S
H1 H 0.892(2) 1.5000 0.264(4) 0.068 Uiso 1 2 d SR
H2 H 0.8799(8) 1.565(7) 0.350(5) 0.068 Uiso 0.50 1 d PR
O1W O 0.4659(5) 0.0000 0.1965(9) 0.135(7) Uani 1 2 d S
H1O1 H 0.4761(16) 0.091(14) 0.231(5) 0.162 Uiso 1 1 d R
O2W O 0.9335(6) 1.6213(7) 0.4876(9) 0.135(9) Uani 0.50 1 d PD
Fe1 Fe 0.64805(7) 1.0000 0.12505(11) 0.0271(4) Uani 1 2 d S
Zn1 Zn 0.5000 0.5000 0.0000 0.0293(5) Uani 1 4 d S
Zn2 Zn 0.79135(5) 1.5000 0.22448(9) 0.0307(4) 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 0.0033 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'
Zn Zn 0.2839 1.4301 '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
N1 C1 Fe1 177.1(8) . .
N2 C2 Fe1 179.3(8) . .
N3 C3 Fe1 178.0(11) . .
N4 C4 Fe1 175.9(12) . .
N5 C5 C7 125.1(13) . .
N5 C5 H5 117.5 . .
C7 C5 H5 117.5 . .
N5 C6 C8 122.9(13) . .
N5 C6 H6 118.6 . .
C8 C6 H6 118.6 . .
C9 C7 C5 116.3(13) . .
C9 C7 H7 121.8 . .
C5 C7 H7 121.8 . .
C9 C8 C6 117.8(13) . .
C9 C8 H8 121.1 . .
C6 C8 H8 121.1 . .
C7 C9 C8 122.0(14) . .
C7 C9 N6 123.1(13) . .
C8 C9 N6 114.9(12) . .
C11 C10 C12 118.0(12) . .
C11 C10 N7 118.4(12) . .
C12 C10 N7 123.5(12) . .
C13 C11 C10 120.7(13) . .
C13 C11 H11 119.7 . .
C10 C11 H11 119.7 . .
C14 C12 C10 116.3(12) . .
C14 C12 H12 121.9 . .
C10 C12 H12 121.9 . .
N8 C13 C11 124.0(12) . .
N8 C13 H13 118.0 . .
C11 C13 H13 118.0 . .
N8 C14 C12 126.3(12) . .
N8 C14 H14 116.8 . .
C12 C14 H14 116.8 . .
C1 N1 Zn1 171.2(7) . .
C2 N2 Zn2 167.4(7) . .
C3 N3 Zn2 168.1(10) . 7_675
C5 N5 C6 115.9(11) . .
C5 N5 Zn1 122.6(8) . .
C6 N5 Zn1 121.5(9) . .
N7 N6 C9 113.6(12) . .
N6 N7 C10 117.3(12) . .
C13 N8 C14 114.7(11) . .
C13 N8 Zn2 129.5(8) . 5_676
C14 N8 Zn2 115.8(8) . 5_676
Zn2 O1 H1 104.8 . .
Zn2 O1 H2 116.3 . .
H1 O1 H2 121.4 . .
C1 Fe1 C1 92.2(5) . 6_575
C1 Fe1 C2 177.5(3) . .
C1 Fe1 C2 90.2(3) 6_575 .
C1 Fe1 C2 90.2(3) . 6_575
C1 Fe1 C2 177.5(3) 6_575 6_575
C2 Fe1 C2 87.4(4) . 6_575
C1 Fe1 C4 87.3(3) . .
C1 Fe1 C4 87.3(3) 6_575 .
C2 Fe1 C4 93.6(3) . .
C2 Fe1 C4 93.6(3) 6_575 .
C1 Fe1 C3 89.4(3) . .
C1 Fe1 C3 89.4(3) 6_575 .
C2 Fe1 C3 89.9(3) . .
C2 Fe1 C3 89.9(3) 6_575 .
C4 Fe1 C3 175.2(5) . .
N1 Zn1 N1 91.0(3) . 6_565
N1 Zn1 N1 180.0(5) . 5_665
N1 Zn1 N1 89.0(3) 6_565 5_665
N1 Zn1 N1 89.0(3) . 2_655
N1 Zn1 N1 180.0(3) 6_565 2_655
N1 Zn1 N1 91.0(3) 5_665 2_655
N1 Zn1 N5 89.5(3) . 5_665
N1 Zn1 N5 89.5(3) 6_565 5_665
N1 Zn1 N5 90.5(3) 5_665 5_665
N1 Zn1 N5 90.5(3) 2_655 5_665
N1 Zn1 N5 90.5(3) . .
N1 Zn1 N5 90.5(3) 6_565 .
N1 Zn1 N5 89.5(3) 5_665 .
N1 Zn1 N5 89.5(3) 2_655 .
N5 Zn1 N5 180.0(4) 5_665 .
N2 Zn2 N2 111.0(4) . 6_585
N2 Zn2 O1 124.32(19) . .
N2 Zn2 O1 124.32(19) 6_585 .
N2 Zn2 N3 93.5(2) . 7_675
N2 Zn2 N3 93.5(2) 6_585 7_675
O1 Zn2 N3 89.1(3) . 7_675
N2 Zn2 N8 86.5(2) . 5_676
N2 Zn2 N8 86.5(2) 6_585 5_676
O1 Zn2 N8 91.0(3) . 5_676
N3 Zn2 N8 179.9(4) 7_675 5_676
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.157(9) .
C1 Fe1 1.915(9) .
C2 N2 1.157(9) .
C2 Fe1 1.919(9) .
C3 N3 1.136(13) .
C3 Fe1 1.957(13) .
C4 N4 1.146(14) .
C4 Fe1 1.942(12) .
C5 N5 1.319(14) .
C5 C7 1.385(16) .
C5 H5 0.9300 .
C6 N5 1.320(14) .
C6 C8 1.373(17) .
C6 H6 0.9300 .
C7 C9 1.308(17) .
C7 H7 0.9300 .
C8 C9 1.356(17) .
C8 H8 0.9300 .
C9 N6 1.509(17) .
C10 C11 1.349(17) .
C10 C12 1.396(15) .
C10 N7 1.422(15) .
C11 C13 1.345(16) .
C11 H11 0.9300 .
C12 C14 1.366(15) .
C12 H12 0.9300 .
C13 N8 1.327(13) .
C13 H13 0.9300 .
C14 N8 1.327(15) .
C14 H14 0.9300 .
N1 Zn1 2.123(7) .
N2 Zn2 2.002(7) .
N3 Zn2 2.075(10) 7_675
N5 Zn1 2.158(9) .
N6 N7 1.149(14) .
N8 Zn2 2.240(10) 5_676
O1 Zn2 2.013(7) .
O1 H1 0.7176 .
O1 H2 0.8066 .
O1W H1O1 0.8422 .
Fe1 C1 1.915(9) 6_575
Fe1 C2 1.919(9) 6_575
Zn1 N1 2.123(7) 6_565
Zn1 N1 2.123(7) 5_665
Zn1 N1 2.123(7) 2_655
Zn1 N5 2.158(9) 5_665
Zn2 N2 2.002(7) 6_585
Zn2 N3 2.075(10) 7_675
Zn2 N8 2.240(10) 5_676
