#------------------------------------------------------------------------------
#$Date: 2015-01-27 21:58:39 +0200 (Tue, 27 Jan 2015) $
#$Revision: 130149 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/06/4000678.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_4000678
loop_
_publ_author_name
'Hyunsoo Park'
'David M. Moureau'
'John B. Parise'
_publ_section_title
;
 Hydrothermal Synthesis and Structural Characterization of Novel
 Zn-Triazole-Benzenedicarboxylate Frameworks
;
_journal_issue                   2
_journal_name_full               'Chem. Mater.'
_journal_page_first              525
_journal_page_last               531
_journal_paper_doi               10.1021/cm051829l
_journal_volume                  18
_journal_year                    2006
_chemical_formula_sum            'C14 H11 N9 O6 Zn2'
_chemical_formula_weight         532.10
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                110.18(3)
_cell_angle_beta                 105.46(3)
_cell_angle_gamma                93.90(3)
_cell_formula_units_Z            2
_cell_length_a                   7.7970(16)
_cell_length_b                   10.047(2)
_cell_length_c                   13.577(3)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      17.68
_cell_measurement_theta_min      1.15
_cell_volume                     947.0(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Endeavor 1.1'
_computing_publication_material  'SHEXL (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2000)'
_computing_structure_solution    'SHELXS (Sheldrick, 2000)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SMART 6000 CCD detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.48595
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13576
_diffrn_reflns_theta_full        17.68
_diffrn_reflns_theta_max         17.68
_diffrn_reflns_theta_min         1.15
_diffrn_source                   synchrotron
_diffrn_source_type              'APS 15-ID beam line'
_exptl_absorpt_coefficient_mu    1.366
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2000)'
_exptl_crystal_colour            coluorless
_exptl_crystal_density_diffrn    1.866
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             540
_exptl_crystal_recrystallization_method hydrothermal
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.353
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         3870
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0345
_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)+(0.0290P)²+4.2388P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.0934
_reflns_number_gt                3720
_reflns_number_total             3870
_reflns_threshold_expression     >2sigma(I)
_cod_database_code               4000678
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Zn1 Zn 0.63082(5) -0.12226(4) 0.25522(3) 0.00516(11) Uani 1 1 d .
Zn2 Zn 1.0000 0.5000 0.5000 0.00509(12) Uani 1 2 d S
Zn3 Zn 1.5000 0.5000 0.5000 0.00524(12) Uani 1 2 d S
O1 O 0.8593(3) -0.0936(3) 0.2098(2) 0.0139(5) Uani 1 1 d .
O2 O 0.6148(4) -0.0929(3) 0.0870(2) 0.0237(6) Uani 1 1 d .
O3 O 0.3642(3) -0.2033(2) 0.1991(2) 0.0103(5) Uani 1 1 d .
O4 O 0.4932(3) -0.3802(3) 0.1126(2) 0.0196(6) Uani 1 1 d .
N1 N 1.0821(4) 0.4272(3) 0.3468(2) 0.0075(5) Uani 1 1 d .
N2 N 1.2607(4) 0.4276(3) 0.3465(2) 0.0080(5) Uani 1 1 d .
N3 N 1.0842(4) 0.3404(3) 0.1764(2) 0.0125(6) Uani 1 1 d .
H3 H 1.0470 0.3032 0.1038 0.015 Uiso 1 1 calc R
N4 N 0.7886(4) 0.3185(3) 0.4303(2) 0.0079(5) Uani 1 1 d .
N5 N 0.6107(4) 0.3141(3) 0.4286(2) 0.0074(5) Uani 1 1 d .
N6 N 0.6489(4) 0.0904(3) 0.3429(2) 0.0091(5) Uani 1 1 d .
N7 N 0.8207(4) 0.6219(3) 0.4350(2) 0.0073(5) Uani 1 1 d .
N8 N 0.6446(4) 0.6211(3) 0.4370(2) 0.0082(5) Uani 1 1 d .
N9 N 0.7022(4) -0.2305(3) 0.3562(2) 0.0091(5) Uani 1 1 d .
C1 C 0.9794(4) 0.3744(4) 0.2436(3) 0.0107(6) Uani 1 1 d .
H1 H 0.8512 0.3618 0.2196 0.013 Uiso 1 1 calc R
C2 C 1.2578(4) 0.3752(4) 0.2435(3) 0.0108(6) Uani 1 1 d .
H2 H 1.3614 0.3633 0.2192 0.013 Uiso 1 1 calc R
C3 C 0.8051(4) 0.1848(3) 0.3787(3) 0.0097(6) Uani 1 1 d .
H3 H 0.9150 0.1575 0.3678 0.012 Uiso 1 1 calc R
C4 C 0.5335(4) 0.1765(3) 0.3761(3) 0.0100(6) Uani 1 1 d .
H4 H 0.4098 0.1422 0.3633 0.012 Uiso 1 1 calc R
C5 C 0.8485(4) 0.7118(3) 0.3865(3) 0.0094(6) Uani 1 1 d .
H5 H 0.9599 0.7333 0.3744 0.011 Uiso 1 1 calc R
C6 C 0.5805(4) 0.7098(4) 0.3897(3) 0.0101(6) Uani 1 1 d .
H6 H 0.4610 0.7294 0.3803 0.012 Uiso 1 1 calc R
C7 C 0.7823(5) -0.0755(4) 0.1221(3) 0.0145(7) Uani 1 1 d .
C8 C 0.8961(5) -0.0361(3) 0.0594(3) 0.0096(6) Uani 1 1 d .
C9 C 1.0818(5) -0.0334(4) 0.0906(3) 0.0110(6) Uani 1 1 d .
H9 H 1.1377 -0.0558 0.1528 0.013 Uiso 1 1 calc R
C10 C 1.1864(5) 0.0020(4) 0.0317(3) 0.0115(6) Uani 1 1 d .
H10 H 1.3130 0.0029 0.0532 0.014 Uiso 1 1 calc R
C11 C 0.0188(4) -0.3756(3) 0.0920(3) 0.0090(6) Uani 1 1 d .
H11 H 0.0322 -0.2908 0.1547 0.011 Uiso 1 1 calc R
C12 C 0.1519(4) -0.5424(4) -0.0303(3) 0.0100(6) Uani 1 1 d .
H12 H 0.2550 -0.5711 -0.0509 0.012 Uiso 1 1 calc R
C13 C 0.1715(4) -0.4173(3) 0.0620(3) 0.0088(6) Uani 1 1 d .
C14 C 0.3567(4) -0.3285(4) 0.1276(3) 0.0110(6) Uani 1 1 d .
O5 O 0.5562(4) -0.6624(3) 0.1186(2) 0.0234(6) Uani 1 1 d .
O6 O 0.1975(7) 0.9251(6) 0.3642(4) 0.0665(13) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 '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 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.3242 0.9375 '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
O3 Zn1 N9 96.57(11) . .
O3 Zn1 N6 104.81(11) . .
N9 Zn1 N6 111.12(12) . .
O3 Zn1 O1 144.84(10) . .
N9 Zn1 O1 103.48(11) . .
N6 Zn1 O1 94.57(11) . .
O3 Zn1 O2 90.74(10) . .
N9 Zn1 O2 150.07(11) . .
N6 Zn1 O2 94.79(11) . .
O1 Zn1 O2 58.15(10) . .
O3 Zn1 C7 118.73(11) . .
N9 Zn1 C7 130.14(12) . .
N6 Zn1 C7 93.59(11) . .
O1 Zn1 C7 29.36(11) . .
O2 Zn1 C7 28.89(11) . .
N4 Zn2 N4 180.0 2_766 .
N4 Zn2 N7 89.68(10) 2_766 .
N4 Zn2 N7 90.32(10) . .
N4 Zn2 N7 90.32(10) 2_766 2_766
N4 Zn2 N7 89.68(10) . 2_766
N7 Zn2 N7 180.00(10) . 2_766
N4 Zn2 N1 90.67(11) 2_766 2_766
N4 Zn2 N1 89.33(11) . 2_766
N7 Zn2 N1 89.43(10) . 2_766
N7 Zn2 N1 90.57(10) 2_766 2_766
N4 Zn2 N1 89.33(11) 2_766 .
N4 Zn2 N1 90.67(11) . .
N7 Zn2 N1 90.57(10) . .
N7 Zn2 N1 89.43(10) 2_766 .
N1 Zn2 N1 179.999(1) 2_766 .
N8 Zn3 N8 180.00(11) 1_655 2_766
N8 Zn3 N5 89.30(10) 1_655 2_766
N8 Zn3 N5 90.70(10) 2_766 2_766
N8 Zn3 N5 90.70(10) 1_655 1_655
N8 Zn3 N5 89.30(10) 2_766 1_655
N5 Zn3 N5 180.000(1) 2_766 1_655
N8 Zn3 N2 88.38(10) 1_655 2_866
N8 Zn3 N2 91.62(10) 2_766 2_866
N5 Zn3 N2 90.17(10) 2_766 2_866
N5 Zn3 N2 89.83(10) 1_655 2_866
N8 Zn3 N2 91.62(10) 1_655 .
N8 Zn3 N2 88.38(10) 2_766 .
N5 Zn3 N2 89.83(10) 2_766 .
N5 Zn3 N2 90.17(10) 1_655 .
N2 Zn3 N2 180.00(12) 2_866 .
C7 O1 Zn1 97.3(2) . .
C7 O2 Zn1 83.7(2) . .
C14 O3 Zn1 102.3(2) . .
C1 N1 N2 107.3(3) . .
C1 N1 Zn2 128.8(2) . .
N2 N1 Zn2 124.0(2) . .
C2 N2 N1 107.3(3) . .
C2 N2 Zn3 128.7(2) . .
N1 N2 Zn3 124.0(2) . .
C1 N3 C2 106.3(3) . .
C3 N4 N5 106.3(3) . .
C3 N4 Zn2 125.2(2) . .
N5 N4 Zn2 128.5(2) . .
C4 N5 N4 105.6(3) . .
C4 N5 Zn3 130.5(2) . 1_455
N4 N5 Zn3 123.9(2) . 1_455
C4 N6 C3 102.5(3) . .
C4 N6 Zn1 135.8(2) . .
C3 N6 Zn1 121.6(2) . .
C5 N7 N8 105.6(3) . .
C5 N7 Zn2 129.8(2) . .
N8 N7 Zn2 124.6(2) . .
C6 N8 N7 106.0(3) . .
C6 N8 Zn3 126.1(2) . 1_455
N7 N8 Zn3 127.8(2) . 1_455
C6 N9 C5 102.7(3) 1_545 1_545
C6 N9 Zn1 121.9(2) 1_545 .
C5 N9 Zn1 133.9(2) 1_545 .
N1 C1 N3 109.5(3) . .
N2 C2 N3 109.6(3) . .
N4 C3 N6 112.8(3) . .
N5 C4 N6 112.9(3) . .
N7 C5 N9 112.8(3) . 1_565
N8 C6 N9 112.9(3) . 1_565
O2 C7 O1 120.5(3) . .
O2 C7 C8 120.5(3) . .
O1 C7 C8 119.0(3) . .
O2 C7 Zn1 67.4(2) . .
O1 C7 Zn1 53.34(17) . .
C8 C7 Zn1 171.1(3) . .
C9 C8 C10 119.8(3) . 2_755
C9 C8 C7 120.9(3) . .
C10 C8 C7 119.3(3) 2_755 .
C10 C9 C8 120.6(3) . .
C9 C10 C8 119.5(3) . 2_755
C12 C11 C13 120.4(3) 2_545 .
C11 C12 C13 119.8(3) 2_545 .
C12 C13 C11 119.8(3) . .
C12 C13 C14 119.4(3) . .
C11 C13 C14 120.7(3) . .
O4 C14 O3 123.6(3) . .
O4 C14 C13 119.5(3) . .
O3 C14 C13 116.8(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O3 2.016(2) .
Zn1 N9 2.019(3) .
Zn1 N6 2.029(3) .
Zn1 O1 2.067(2) .
Zn1 O2 2.374(3) .
Zn1 C7 2.556(4) .
Zn2 N4 2.123(3) 2_766
Zn2 N4 2.123(3) .
Zn2 N7 2.134(3) .
Zn2 N7 2.134(3) 2_766
Zn2 N1 2.235(3) 2_766
Zn2 N1 2.235(3) .
Zn3 N8 2.128(3) 1_655
Zn3 N8 2.128(3) 2_766
Zn3 N5 2.142(3) 2_766
Zn3 N5 2.142(3) 1_655
Zn3 N2 2.247(3) 2_866
Zn3 N2 2.247(3) .
O1 C7 1.263(5) .
O2 C7 1.242(5) .
O3 C14 1.283(4) .
O4 C14 1.250(4) .
N1 C1 1.309(4) .
N1 N2 1.393(4) .
N2 C2 1.306(4) .
N3 C1 1.355(4) .
N3 C2 1.358(4) .
N4 C3 1.318(4) .
N4 N5 1.379(4) .
N5 C4 1.327(4) .
N5 Zn3 2.142(3) 1_455
N6 C4 1.347(4) .
N6 C3 1.352(4) .
N7 C5 1.326(4) .
N7 N8 1.380(4) .
N8 C6 1.319(4) .
N8 Zn3 2.128(3) 1_455
N9 C6 1.344(4) 1_545
N9 C5 1.345(4) 1_545
C5 N9 1.345(4) 1_565
C6 N9 1.344(4) 1_565
C7 C8 1.502(5) .
C8 C9 1.391(5) .
C8 C10 1.400(5) 2_755
C9 C10 1.391(5) .
C10 C8 1.400(5) 2_755
C11 C12 1.390(5) 2_545
C11 C13 1.402(5) .
C12 C11 1.390(5) 2_545
C12 C13 1.400(5) .
C13 C14 1.505(4) .
