#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:40:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179198 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/36/4313608.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_4313608
loop_
_publ_author_name
'Jian Fan'
'Wei-Yin Sun'
'Taka-aki Okamura'
'Wen-Xia Tang'
'Norikazu Ueyama'
_publ_section_title
;
 Novel Metal-Organic Frameworks with Specific Topology from New Tripodal
 Ligands: 1,3,5-Tris(1-imidazolyl)benzene and
 1,3-Bis(1-imidazolyl)-5-(imidazol-1-ylmethyl)benzene
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3168
_journal_page_last               3175
_journal_paper_doi               10.1021/ic0206847
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C30 H28 N14 O8 Zn '
_chemical_formula_sum            'C30 H28 N14 O8 Zn'
_chemical_formula_weight         778.03
_chemical_name_systematic
;
[Zn(4)2(H2O)2](NO3)2
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             'Sun Jun 30 14:30:06 2002'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.2779(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.5699(3)
_cell_length_b                   11.5037(3)
_cell_length_c                   13.5194(4)
_cell_measurement_reflns_used    10942
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.7
_cell_volume                     1541.98(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14692
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.876
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         3510
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0395P)²+0.3679P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0702
_refine_ls_wR_factor_ref         0.0733
_reflns_number_gt                2829
_reflns_number_total             3510
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0206847_4.cif
_cod_data_source_block           9
_cod_original_cell_volume        1541.98(7)
_cod_database_code               4313608
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.5000 0.0000 0.5000 0.01437(8) Uani 1 2 d S . .
O1 O 0.65471(14) 0.05159(13) 0.64865(11) 0.0242(3) Uani 1 1 d . . .
H13 H 0.723(2) 0.016(2) 0.6702(18) 0.029 Uiso 1 1 d . . .
H14 H 0.666(2) 0.116(2) 0.6663(17) 0.029 Uiso 1 1 d . . .
O11 O 0.55533(17) 0.23922(14) 0.78825(12) 0.0427(4) Uani 1 1 d . . .
O12 O 0.60883(15) 0.41981(14) 0.79793(16) 0.0508(5) Uani 1 1 d . . .
O13 O 0.67322(17) 0.30367(17) 0.69989(13) 0.0506(5) Uani 1 1 d . . .
N1 N 0.61394(14) 0.32113(14) 0.76263(12) 0.0225(3) Uani 1 1 d . . .
N11 N 0.64440(13) -0.34775(12) 0.50328(11) 0.0154(3) Uani 1 1 d . . .
N12 N 0.56056(14) -0.17805(12) 0.52479(11) 0.0166(3) Uani 1 1 d . . .
N31 N 0.28800(14) -0.02544(11) 0.71798(10) 0.0140(3) Uani 1 1 d . . .
N32 N 0.36534(14) -0.02587(11) 0.58612(11) 0.0154(3) Uani 1 1 d . . .
N51 N 0.93920(14) -0.68360(12) 0.54951(11) 0.0152(3) Uani 1 1 d . . .
N52 N 1.10093(15) -0.81666(14) 0.60600(12) 0.0230(3) Uani 1 1 d . . .
C1 C 0.71360(16) -0.43057(14) 0.46223(13) 0.0151(3) Uani 1 1 d . . .
C2 C 0.71066(16) -0.41589(14) 0.35925(13) 0.0156(3) Uani 1 1 d . . .
H1 H 0.6591 -0.3553 0.3161 0.019 Uiso 1 1 calc R . .
C3 C 0.78458(15) -0.49150(15) 0.32138(12) 0.0143(3) Uani 1 1 d . . .
C4 C 0.85574(16) -0.58318(15) 0.38202(13) 0.0156(3) Uani 1 1 d . . .
H2 H 0.9019 -0.6372 0.3535 0.019 Uiso 1 1 calc R . .
C5 C 0.85855(16) -0.59498(14) 0.48519(13) 0.0140(3) Uani 1 1 d . . .
C6 C 0.78722(16) -0.51882(14) 0.52660(13) 0.0162(3) Uani 1 1 d . . .
H3 H 0.7890 -0.5271 0.5970 0.019 Uiso 1 1 calc R . .
C11 C 0.63460(17) -0.23297(15) 0.47893(13) 0.0168(3) Uani 1 1 d . . .
H4 H 0.6758 -0.1969 0.4346 0.020 Uiso 1 1 calc R . .
C12 C 0.52138(18) -0.26194(16) 0.58162(14) 0.0213(4) Uani 1 1 d . . .
H5 H 0.4661 -0.2481 0.6228 0.026 Uiso 1 1 calc R . .
C13 C 0.57317(18) -0.36660(16) 0.57011(13) 0.0204(4) Uani 1 1 d . . .
H6 H 0.5626 -0.4381 0.6015 0.024 Uiso 1 1 calc R . .
C31 C 0.39199(16) 0.00211(15) 0.68576(13) 0.0158(3) Uani 1 1 d . . .
H7 H 0.4737 0.0371 0.7294 0.019 Uiso 1 1 calc R . .
C32 C 0.23715(17) -0.07326(15) 0.55254(14) 0.0197(4) Uani 1 1 d . . .
H8 H 0.1901 -0.1010 0.4833 0.024 Uiso 1 1 calc R . .
C33 C 0.18875(17) -0.07429(15) 0.63298(13) 0.0191(4) Uani 1 1 d . . .
H9 H 0.1037 -0.1029 0.6313 0.023 Uiso 1 1 calc R . .
C51 C 1.03869(16) -0.74501(15) 0.52943(13) 0.0173(3) Uani 1 1 d . . .
H10 H 1.0600 -0.7366 0.4671 0.021 Uiso 1 1 calc R . .
C52 C 1.03803(19) -0.80265(16) 0.67892(14) 0.0228(4) Uani 1 1 d . . .
H11 H 1.0609 -0.8445 0.7433 0.027 Uiso 1 1 calc R . .
C53 C 0.93902(18) -0.72118(16) 0.64679(13) 0.0200(4) Uani 1 1 d . . .
H12 H 0.8819 -0.6955 0.6833 0.024 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Zn Zn 0.2839 1.4301 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
_geom_angle_publ_flag
N12 Zn1 N12 179.999(1) . 3_656 ?
N12 Zn1 N32 89.95(5) . 3_656 ?
N12 Zn1 N32 90.05(5) 3_656 3_656 ?
N12 Zn1 N32 90.05(5) . . ?
N12 Zn1 N32 89.95(5) 3_656 . ?
N32 Zn1 N32 180.0 3_656 . ?
N12 Zn1 O1 88.39(5) . 3_656 ?
N12 Zn1 O1 91.61(5) 3_656 3_656 ?
N32 Zn1 O1 87.97(5) 3_656 3_656 ?
N32 Zn1 O1 92.03(5) . 3_656 ?
N12 Zn1 O1 91.61(5) . . ?
N12 Zn1 O1 88.39(5) 3_656 . ?
N32 Zn1 O1 92.03(5) 3_656 . ?
N32 Zn1 O1 87.96(5) . . ?
O1 Zn1 O1 180.0 3_656 . ?
Zn1 O1 H13 119.8(17) . . ?
Zn1 O1 H14 121.8(16) . . ?
H13 O1 H14 111(2) . . ?
O13 N1 O12 120.94(18) . . ?
O13 N1 O11 119.34(17) . . ?
O12 N1 O11 119.68(17) . . ?
C11 N11 C13 107.40(14) . . ?
C11 N11 C1 124.24(14) . . ?
C13 N11 C1 128.34(14) . . ?
C11 N12 C12 105.55(14) . . ?
C11 N12 Zn1 125.50(12) . . ?
C12 N12 Zn1 128.65(11) . . ?
C31 N31 C33 107.19(14) . . ?
C31 N31 C3 125.72(14) . 4_556 ?
C33 N31 C3 127.08(14) . 4_556 ?
C31 N32 C32 105.67(14) . . ?
C31 N32 Zn1 124.97(11) . . ?
C32 N32 Zn1 129.36(11) . . ?
C51 N51 C53 106.32(14) . . ?
C51 N51 C5 126.10(14) . . ?
C53 N51 C5 127.50(14) . . ?
C51 N52 C52 104.94(15) . . ?
C6 C1 C2 121.97(15) . . ?
C6 C1 N11 119.79(15) . . ?
C2 C1 N11 118.14(14) . . ?
C3 C2 C1 118.36(15) . . ?
C3 C2 H1 120.8 . . ?
C1 C2 H1 120.8 . . ?
C2 C3 C4 121.38(15) . . ?
C2 C3 N31 119.20(15) . 4_655 ?
C4 C3 N31 119.42(14) . 4_655 ?
C3 C4 C5 119.05(15) . . ?
C3 C4 H2 120.5 . . ?
C5 C4 H2 120.5 . . ?
C4 C5 C6 120.99(15) . . ?
C4 C5 N51 118.99(14) . . ?
C6 C5 N51 119.99(14) . . ?
C1 C6 C5 118.17(15) . . ?
C1 C6 H3 120.9 . . ?
C5 C6 H3 120.9 . . ?
N12 C11 N11 111.16(15) . . ?
N12 C11 H4 124.4 . . ?
N11 C11 H4 124.4 . . ?
C13 C12 N12 110.23(15) . . ?
C13 C12 H5 124.9 . . ?
N12 C12 H5 124.9 . . ?
C12 C13 N11 105.65(15) . . ?
C12 C13 H6 127.2 . . ?
N11 C13 H6 127.2 . . ?
N32 C31 N31 111.25(14) . . ?
N32 C31 H7 124.4 . . ?
N31 C31 H7 124.4 . . ?
C33 C32 N32 109.87(15) . . ?
C33 C32 H8 125.1 . . ?
N32 C32 H8 125.1 . . ?
C32 C33 N31 106.02(15) . . ?
C32 C33 H9 127.0 . . ?
N31 C33 H9 127.0 . . ?
N52 C51 N51 112.22(15) . . ?
N52 C51 H10 123.9 . . ?
N51 C51 H10 123.9 . . ?
C53 C52 N52 111.19(15) . . ?
C53 C52 H11 124.4 . . ?
N52 C52 H11 124.4 . . ?
C52 C53 N51 105.33(15) . . ?
C52 C53 H12 127.3 . . ?
N51 C53 H12 127.3 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 N12 2.1375(14) . ?
Zn1 N12 2.1375(14) 3_656 ?
Zn1 N32 2.1491(14) 3_656 ?
Zn1 N32 2.1491(14) . ?
Zn1 O1 2.1879(13) 3_656 ?
Zn1 O1 2.1880(13) . ?
O1 H13 0.79(2) . ?
O1 H14 0.78(2) . ?
O11 N1 1.241(2) . ?
O12 N1 1.240(2) . ?
O13 N1 1.233(2) . ?
N11 C11 1.356(2) . ?
N11 C13 1.379(2) . ?
N11 C1 1.426(2) . ?
N12 C11 1.316(2) . ?
N12 C12 1.383(2) . ?
N31 C31 1.353(2) . ?
N31 C33 1.379(2) . ?
N31 C3 1.424(2) 4_556 ?
N32 C31 1.317(2) . ?
N32 C32 1.383(2) . ?
N51 C51 1.370(2) . ?
N51 C53 1.385(2) . ?
N51 C5 1.417(2) . ?
N52 C51 1.308(2) . ?
N52 C52 1.376(2) . ?
C1 C6 1.387(2) . ?
C1 C2 1.392(2) . ?
C2 C3 1.381(2) . ?
C2 H1 0.9500 . ?
C3 C4 1.387(2) . ?
C3 N31 1.424(2) 4_655 ?
C4 C5 1.391(2) . ?
C4 H2 0.9500 . ?
C5 C6 1.394(2) . ?
C6 H3 0.9500 . ?
C11 H4 0.9500 . ?
C12 C13 1.354(2) . ?
C12 H5 0.9500 . ?
C13 H6 0.9500 . ?
C31 H7 0.9500 . ?
C32 C33 1.353(2) . ?
C32 H8 0.9500 . ?
C33 H9 0.9500 . ?
C51 H10 0.9500 . ?
C52 C53 1.359(2) . ?
C52 H11 0.9500 . ?
C53 H12 0.9500 . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N12 Zn1 N12 C11 -135(10) 3_656 . . . ?
N32 Zn1 N12 C11 -9.99(14) 3_656 . . . ?
N32 Zn1 N12 C11 170.02(14) . . . . ?
O1 Zn1 N12 C11 77.98(14) 3_656 . . . ?
O1 Zn1 N12 C11 -102.02(14) . . . . ?
N12 Zn1 N12 C12 52(10) 3_656 . . . ?
N32 Zn1 N12 C12 177.18(15) 3_656 . . . ?
N32 Zn1 N12 C12 -2.82(15) . . . . ?
O1 Zn1 N12 C12 -94.85(15) 3_656 . . . ?
O1 Zn1 N12 C12 85.14(15) . . . . ?
N12 Zn1 N32 C31 98.92(14) . . . . ?
N12 Zn1 N32 C31 -81.08(14) 3_656 . . . ?
N32 Zn1 N32 C31 -18(3) 3_656 . . . ?
O1 Zn1 N32 C31 -172.68(14) 3_656 . . . ?
O1 Zn1 N32 C31 7.32(14) . . . . ?
N12 Zn1 N32 C32 -81.02(15) . . . . ?
N12 Zn1 N32 C32 98.98(15) 3_656 . . . ?
N32 Zn1 N32 C32 162(3) 3_656 . . . ?
O1 Zn1 N32 C32 7.38(15) 3_656 . . . ?
O1 Zn1 N32 C32 -172.62(15) . . . . ?
C11 N11 C1 C6 141.88(17) . . . . ?
C13 N11 C1 C6 -40.3(2) . . . . ?
C11 N11 C1 C2 -34.7(2) . . . . ?
C13 N11 C1 C2 143.19(17) . . . . ?
C6 C1 C2 C3 -0.5(2) . . . . ?
N11 C1 C2 C3 175.93(14) . . . . ?
C1 C2 C3 C4 2.7(2) . . . . ?
C1 C2 C3 N31 -177.05(14) . . . 4_655 ?
C2 C3 C4 C5 -3.7(2) . . . . ?
N31 C3 C4 C5 176.14(14) 4_655 . . . ?
C3 C4 C5 C6 2.3(2) . . . . ?
C3 C4 C5 N51 -175.47(14) . . . . ?
C51 N51 C5 C4 15.0(2) . . . . ?
C53 N51 C5 C4 -168.78(16) . . . . ?
C51 N51 C5 C6 -162.85(16) . . . . ?
C53 N51 C5 C6 13.4(2) . . . . ?
C2 C1 C6 C5 -0.7(2) . . . . ?
N11 C1 C6 C5 -177.11(14) . . . . ?
C4 C5 C6 C1 -0.2(2) . . . . ?
N51 C5 C6 C1 177.58(14) . . . . ?
C12 N12 C11 N11 0.19(19) . . . . ?
Zn1 N12 C11 N11 -174.01(10) . . . . ?
C13 N11 C11 N12 -0.78(19) . . . . ?
C1 N11 C11 N12 177.45(14) . . . . ?
C11 N12 C12 C13 0.5(2) . . . . ?
Zn1 N12 C12 C13 174.44(12) . . . . ?
N12 C12 C13 N11 -0.9(2) . . . . ?
C11 N11 C13 C12 1.03(19) . . . . ?
C1 N11 C13 C12 -177.10(16) . . . . ?
C32 N32 C31 N31 0.35(19) . . . . ?
Zn1 N32 C31 N31 -179.60(10) . . . . ?
C33 N31 C31 N32 0.05(19) . . . . ?
C3 N31 C31 N32 178.96(14) 4_556 . . . ?
C31 N32 C32 C33 -0.6(2) . . . . ?
Zn1 N32 C32 C33 179.31(12) . . . . ?
N32 C32 C33 N31 0.7(2) . . . . ?
C31 N31 C33 C32 -0.44(19) . . . . ?
C3 N31 C33 C32 -179.34(15) 4_556 . . . ?
C52 N52 C51 N51 0.8(2) . . . . ?
C53 N51 C51 N52 -0.5(2) . . . . ?
C5 N51 C51 N52 176.37(15) . . . . ?
C51 N52 C52 C53 -0.9(2) . . . . ?
N52 C52 C53 N51 0.6(2) . . . . ?
C51 N51 C53 C52 -0.06(19) . . . . ?
C5 N51 C53 C52 -176.88(15) . . . . ?
