#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:40:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179198 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/36/4313607.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_4313607
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         'C34 H38 Cu N12 O8 '
_chemical_formula_sum            'C34 H38 Cu N12 O8'
_chemical_formula_weight         806.30
_chemical_name_systematic
;
[Cu(4)2](OAc)2-4(H2O)
;
_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             'Tue Nov 13 19:12:44 2001'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.5740(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.2969(5)
_cell_length_b                   12.2834(5)
_cell_length_c                   17.4667(12)
_cell_measurement_reflns_used    14597
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.0
_cell_volume                     1768.40(18)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0639
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16745
_diffrn_reflns_theta_full        27.41
_diffrn_reflns_theta_max         27.41
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.689
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             838
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4011
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0396
_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)+(0.0539P)²+0.2173P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0937
_reflns_number_gt                3218
_reflns_number_total             4011
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0206847_3.cif
_cod_data_source_block           8
_cod_database_code               4313607
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
Cu1 Cu 1.0000 0.0000 0.5000 0.01334(10) Uani 1 2 d S . .
O1 O 0.77327(19) 0.10606(11) 0.71382(9) 0.0336(4) Uani 1 1 d . . .
O2 O 0.87896(19) 0.26995(12) 0.70331(11) 0.0392(4) Uani 1 1 d . . .
O3 O 0.8004(2) 0.48455(14) 0.65807(10) 0.0379(4) Uani 1 1 d . . .
H16 H 0.817(3) 0.424(2) 0.6710(17) 0.046 Uiso 1 1 d . . .
H17 H 0.767(3) 0.519(2) 0.6924(18) 0.046 Uiso 1 1 d . . .
O4 O 0.76805(18) -0.00196(12) 0.57004(9) 0.0254(3) Uani 1 1 d . . .
H18 H 0.753(3) 0.0241(19) 0.6106(16) 0.030 Uiso 1 1 d . . .
H19 H 0.726(3) -0.058(2) 0.5646(15) 0.030 Uiso 1 1 d . . .
N11 N 1.23717(18) -0.01308(11) 0.72286(9) 0.0165(3) Uani 1 1 d . . .
N12 N 1.14847(18) -0.00388(10) 0.59954(9) 0.0155(3) Uani 1 1 d . . .
N31 N 1.39445(18) -0.17012(11) 0.97384(9) 0.0154(3) Uani 1 1 d . . .
N32 N 1.48707(18) -0.33461(12) 1.00389(9) 0.0160(3) Uani 1 1 d . . .
N51 N 1.07017(18) 0.16059(11) 0.95003(9) 0.0177(3) Uani 1 1 d . . .
N52 N 0.9029(2) 0.29896(13) 0.96037(10) 0.0246(4) Uani 1 1 d . . .
C1 C 1.2351(2) -0.00953(13) 0.80402(10) 0.0162(4) Uani 1 1 d . . .
C2 C 1.3188(2) -0.08923(13) 0.84902(11) 0.0167(4) Uani 1 1 d . . .
H1 H 1.3781 -0.1443 0.8262 0.020 Uiso 1 1 calc R . .
C3 C 1.3134(2) -0.08621(13) 0.92781(11) 0.0152(4) Uani 1 1 d . . .
C4 C 1.2287(2) -0.00613(13) 0.96294(10) 0.0166(4) Uani 1 1 d . . .
H2 H 1.2240 -0.0062 1.0170 0.020 Uiso 1 1 calc R . .
C5 C 1.1506(2) 0.07435(13) 0.91579(11) 0.0155(4) Uani 1 1 d . . .
C6 C 1.1530(2) 0.07341(14) 0.83653(11) 0.0178(4) Uani 1 1 d . . .
H3 H 1.0992 0.1286 0.8052 0.021 Uiso 1 1 calc R . .
C7 C 0.7668(2) 0.20816(16) 0.71574(11) 0.0227(4) Uani 1 1 d . . .
C8 C 0.6115(3) 0.2587(2) 0.73711(15) 0.0409(6) Uani 1 1 d . . .
H13 H 0.5361 0.2010 0.7483 0.049 Uiso 1 1 calc R . .
H14 H 0.5619 0.3031 0.6941 0.049 Uiso 1 1 calc R . .
H15 H 0.6361 0.3047 0.7828 0.049 Uiso 1 1 calc R . .
C11 C 1.1104(2) 0.01185(12) 0.66985(11) 0.0157(4) Uani 1 1 d . . .
H4 H 1.0080 0.0372 0.6818 0.019 Uiso 1 1 calc R . .
C12 C 1.3068(2) -0.04048(16) 0.60736(11) 0.0209(4) Uani 1 1 d . . .
H5 H 1.3670 -0.0581 0.5660 0.025 Uiso 1 1 calc R . .
C13 C 1.3629(2) -0.04744(17) 0.68301(11) 0.0246(4) Uani 1 1 d . . .
H6 H 1.4674 -0.0711 0.7045 0.029 Uiso 1 1 calc R . .
C31 C 1.4163(2) -0.27277(14) 0.94861(11) 0.0176(4) Uani 1 1 d . . .
H7 H 1.3844 -0.2969 0.8975 0.021 Uiso 1 1 calc R . .
C32 C 1.5124(2) -0.26775(14) 1.06805(11) 0.0177(4) Uani 1 1 d . . .
H8 H 1.5630 -0.2897 1.1172 0.021 Uiso 1 1 calc R . .
C33 C 1.4545(2) -0.16680(14) 1.05066(11) 0.0178(4) Uani 1 1 d . . .
H9 H 1.4551 -0.1061 1.0844 0.021 Uiso 1 1 calc R . .
C51 C 0.9460(2) 0.22200(15) 0.91518(12) 0.0241(4) Uani 1 1 d . . .
H10 H 0.8965 0.2103 0.8641 0.029 Uiso 1 1 calc R . .
C52 C 1.0037(2) 0.28675(16) 1.02815(13) 0.0255(4) Uani 1 1 d . . .
H11 H 1.0009 0.3313 1.0724 0.031 Uiso 1 1 calc R . .
C53 C 1.1070(3) 0.20283(16) 1.02304(12) 0.0265(4) Uani 1 1 d . . .
H12 H 1.1883 0.1780 1.0618 0.032 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
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'
Cu Cu 0.3201 1.2651 '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 Cu1 N12 179.999(1) . 3_756 ?
N12 Cu1 N32 88.68(5) . 4 ?
N12 Cu1 N32 91.32(5) 3_756 4 ?
N12 Cu1 N32 91.32(5) . 2_756 ?
N12 Cu1 N32 88.68(5) 3_756 2_756 ?
N32 Cu1 N32 180.0 4 2_756 ?
N12 Cu1 O4 90.38(6) . . ?
N12 Cu1 O4 89.62(6) 3_756 . ?
N32 Cu1 O4 85.67(5) 4 . ?
N32 Cu1 O4 94.33(5) 2_756 . ?
N12 Cu1 O4 89.62(6) . 3_756 ?
N12 Cu1 O4 90.38(6) 3_756 3_756 ?
N32 Cu1 O4 94.33(5) 4 3_756 ?
N32 Cu1 O4 85.67(5) 2_756 3_756 ?
O4 Cu1 O4 180.0 . 3_756 ?
H16 O3 H17 110(3) . . ?
Cu1 O4 H18 131.3(18) . . ?
Cu1 O4 H19 109.2(18) . . ?
H18 O4 H19 111(2) . . ?
C11 N11 C13 107.22(16) . . ?
C11 N11 C1 125.34(16) . . ?
C13 N11 C1 127.36(15) . . ?
C11 N12 C12 106.41(15) . . ?
C11 N12 Cu1 127.86(13) . . ?
C12 N12 Cu1 125.07(13) . . ?
C31 N31 C33 107.31(14) . . ?
C31 N31 C3 124.11(15) . . ?
C33 N31 C3 128.46(14) . . ?
C31 N32 C32 105.39(15) . . ?
C31 N32 Cu1 125.00(12) . 2_746 ?
C32 N32 Cu1 127.93(12) . 2_746 ?
C51 N51 C53 106.31(15) . . ?
C51 N51 C5 126.34(16) . . ?
C53 N51 C5 127.26(16) . . ?
C51 N52 C52 105.06(15) . . ?
C6 C1 C2 121.61(17) . . ?
C6 C1 N11 119.67(15) . . ?
C2 C1 N11 118.72(15) . . ?
C3 C2 C1 118.22(16) . . ?
C3 C2 H1 120.9 . . ?
C1 C2 H1 120.9 . . ?
C2 C3 C4 122.23(16) . . ?
C2 C3 N31 118.33(15) . . ?
C4 C3 N31 119.42(16) . . ?
C3 C4 C5 117.62(16) . . ?
C3 C4 H2 121.2 . . ?
C5 C4 H2 121.2 . . ?
C6 C5 C4 121.61(16) . . ?
C6 C5 N51 119.18(15) . . ?
C4 C5 N51 119.20(16) . . ?
C1 C6 C5 118.66(16) . . ?
C1 C6 H3 120.7 . . ?
C5 C6 H3 120.7 . . ?
O2 C7 O1 124.84(19) . . ?
O2 C7 C8 118.00(19) . . ?
O1 C7 C8 117.13(19) . . ?
C7 C8 H13 109.5 . . ?
C7 C8 H14 109.5 . . ?
H13 C8 H14 109.5 . . ?
C7 C8 H15 109.5 . . ?
H13 C8 H15 109.5 . . ?
H14 C8 H15 109.5 . . ?
N12 C11 N11 110.74(16) . . ?
N12 C11 H4 124.6 . . ?
N11 C11 H4 124.6 . . ?
C13 C12 N12 109.56(17) . . ?
C13 C12 H5 125.2 . . ?
N12 C12 H5 125.2 . . ?
C12 C13 N11 106.06(16) . . ?
C12 C13 H6 127.0 . . ?
N11 C13 H6 127.0 . . ?
N32 C31 N31 111.37(16) . . ?
N32 C31 H7 124.3 . . ?
N31 C31 H7 124.3 . . ?
C33 C32 N32 110.18(16) . . ?
C33 C32 H8 124.9 . . ?
N32 C32 H8 124.9 . . ?
C32 C33 N31 105.74(15) . . ?
C32 C33 H9 127.1 . . ?
N31 C33 H9 127.1 . . ?
N52 C51 N51 112.04(18) . . ?
N52 C51 H10 124.0 . . ?
N51 C51 H10 124.0 . . ?
C53 C52 N52 110.71(18) . . ?
C53 C52 H11 124.6 . . ?
N52 C52 H11 124.6 . . ?
C52 C53 N51 105.88(18) . . ?
C52 C53 H12 127.1 . . ?
N51 C53 H12 127.1 . . ?
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
Cu1 N12 2.0130(15) . ?
Cu1 N12 2.0130(15) 3_756 ?
Cu1 N32 2.0359(14) 4 ?
Cu1 N32 2.0360(14) 2_756 ?
Cu1 O4 2.3958(15) . ?
Cu1 O4 2.3958(15) 3_756 ?
O1 C7 1.256(2) . ?
O2 C7 1.239(2) . ?
O3 H16 0.78(3) . ?
O3 H17 0.81(3) . ?
O4 H18 0.80(3) . ?
O4 H19 0.77(2) . ?
N11 C11 1.354(2) . ?
N11 C13 1.385(2) . ?
N11 C1 1.420(2) . ?
N12 C11 1.317(2) . ?
N12 C12 1.380(2) . ?
N31 C31 1.355(2) . ?
N31 C33 1.377(2) . ?
N31 C3 1.427(2) . ?
N32 C31 1.313(2) . ?
N32 C32 1.386(2) . ?
N32 Cu1 2.0359(14) 2_746 ?
N51 C51 1.363(2) . ?
N51 C53 1.378(2) . ?
N51 C5 1.420(2) . ?
N52 C51 1.307(3) . ?
N52 C52 1.377(3) . ?
C1 C6 1.383(2) . ?
C1 C2 1.390(2) . ?
C2 C3 1.383(3) . ?
C2 H1 0.9500 . ?
C3 C4 1.392(2) . ?
C4 C5 1.397(2) . ?
C4 H2 0.9500 . ?
C5 C6 1.387(3) . ?
C6 H3 0.9500 . ?
C7 C8 1.514(3) . ?
C8 H13 0.9800 . ?
C8 H14 0.9800 . ?
C8 H15 0.9800 . ?
C11 H4 0.9500 . ?
C12 C13 1.352(3) . ?
C12 H5 0.9500 . ?
C13 H6 0.9500 . ?
C31 H7 0.9500 . ?
C32 C33 1.352(2) . ?
C32 H8 0.9500 . ?
C33 H9 0.9500 . ?
C51 H10 0.9500 . ?
C52 C53 1.350(3) . ?
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 Cu1 N12 C11 160(4) 3_756 . . . ?
N32 Cu1 N12 C11 -98.03(14) 4 . . . ?
N32 Cu1 N12 C11 81.97(14) 2_756 . . . ?
O4 Cu1 N12 C11 -12.37(14) . . . . ?
O4 Cu1 N12 C11 167.63(14) 3_756 . . . ?
N12 Cu1 N12 C12 -31(4) 3_756 . . . ?
N32 Cu1 N12 C12 71.33(15) 4 . . . ?
N32 Cu1 N12 C12 -108.67(15) 2_756 . . . ?
O4 Cu1 N12 C12 156.98(15) . . . . ?
O4 Cu1 N12 C12 -23.02(15) 3_756 . . . ?
C11 N11 C1 C6 -38.7(2) . . . . ?
C13 N11 C1 C6 144.96(19) . . . . ?
C11 N11 C1 C2 142.32(17) . . . . ?
C13 N11 C1 C2 -34.0(3) . . . . ?
C6 C1 C2 C3 2.3(3) . . . . ?
N11 C1 C2 C3 -178.77(16) . . . . ?
C1 C2 C3 C4 -0.5(3) . . . . ?
C1 C2 C3 N31 177.83(15) . . . . ?
C31 N31 C3 C2 -29.3(3) . . . . ?
C33 N31 C3 C2 155.25(17) . . . . ?
C31 N31 C3 C4 149.10(18) . . . . ?
C33 N31 C3 C4 -26.4(3) . . . . ?
C2 C3 C4 C5 -1.5(3) . . . . ?
N31 C3 C4 C5 -179.82(15) . . . . ?
C3 C4 C5 C6 1.8(3) . . . . ?
C3 C4 C5 N51 -176.71(16) . . . . ?
C51 N51 C5 C6 25.7(3) . . . . ?
C53 N51 C5 C6 -150.48(19) . . . . ?
C51 N51 C5 C4 -155.76(18) . . . . ?
C53 N51 C5 C4 28.1(3) . . . . ?
C2 C1 C6 C5 -2.0(3) . . . . ?
N11 C1 C6 C5 179.07(16) . . . . ?
C4 C5 C6 C1 -0.1(3) . . . . ?
N51 C5 C6 C1 178.42(16) . . . . ?
C12 N12 C11 N11 -0.05(18) . . . . ?
Cu1 N12 C11 N11 170.88(10) . . . . ?
C13 N11 C11 N12 -0.40(19) . . . . ?
C1 N11 C11 N12 -177.31(14) . . . . ?
C11 N12 C12 C13 0.5(2) . . . . ?
Cu1 N12 C12 C13 -170.75(13) . . . . ?
N12 C12 C13 N11 -0.7(2) . . . . ?
C11 N11 C13 C12 0.7(2) . . . . ?
C1 N11 C13 C12 177.52(16) . . . . ?
C32 N32 C31 N31 -0.2(2) . . . . ?
Cu1 N32 C31 N31 165.98(12) 2_746 . . . ?
C33 N31 C31 N32 -0.5(2) . . . . ?
C3 N31 C31 N32 -176.75(16) . . . . ?
C31 N32 C32 C33 0.7(2) . . . . ?
Cu1 N32 C32 C33 -164.84(13) 2_746 . . . ?
N32 C32 C33 N31 -1.0(2) . . . . ?
C31 N31 C33 C32 0.9(2) . . . . ?
C3 N31 C33 C32 176.97(17) . . . . ?
C52 N52 C51 N51 -0.3(2) . . . . ?
C53 N51 C51 N52 0.2(2) . . . . ?
C5 N51 C51 N52 -176.63(17) . . . . ?
C51 N52 C52 C53 0.3(2) . . . . ?
N52 C52 C53 N51 -0.2(2) . . . . ?
C51 N51 C53 C52 0.0(2) . . . . ?
C5 N51 C53 C52 176.78(17) . . . . ?
