# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2009
data_global
_journal_coden_Cambridge 222
loop_
_publ_author_name
'Christoph Janiak'
'Hesham A Habib'
'Anke Hoffmann'
'Henning A. Hoppe'
_publ_contact_author_name 'Christoph Janiak'
_publ_contact_author_email JANIAK@UNI-FREIBURG.DE
_publ_section_title
;
Crystal structures and solid-state CPMAS 13C NMR
correlations in luminescent zinc(II) and cadmium(II) mixed-ligand
coordination polymers constructed from
1,2-bis(1,2,4-triazol-4-yl)ethane and benzenedicarboxylate
;
# Attachment '1.CIF'
data_35-znfin
_database_code_depnum_ccdc_archive 'CCDC 695986'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
catena-[(\m2-benzene-1,4-dicarboxylato-\k2O,O':\k2O'',O''')-
(\m2-benzene-1,4-dicarboxylato-\kO:\kO'')-
(\m4-1,2-bis(1,2,4-triazol-4-yl)ethane-\kN1:\kN1':\kN2':\kN2')-dizinc(II)]
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C11 H8 N3 O4 Zn'
_chemical_formula_sum 'C11 H8 N3 O4 Zn'
_chemical_formula_weight 311.59
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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M C2/c
_symmetry_space_group_name_Hall '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 12.4552(10)
_cell_length_b 15.1581(10)
_cell_length_c 13.274(2)
_cell_angle_alpha 90.00
_cell_angle_beta 117.432(10)
_cell_angle_gamma 90.00
_cell_volume 2224.3(4)
_cell_formula_units_Z 8
_cell_measurement_temperature 203(2)
_cell_measurement_reflns_used 8963
_cell_measurement_theta_min 2.28
_cell_measurement_theta_max 38.6
_exptl_crystal_description parallelepiped
_exptl_crystal_colour colorless
_exptl_crystal_size_max 0.60
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.20
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.861
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1256
_exptl_absorpt_coefficient_mu 2.223
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.3349
_exptl_absorpt_correction_T_max 0.6382
_exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 203(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker APEX2 CCD area detector'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 46785
_diffrn_reflns_av_R_equivalents 0.0288
_diffrn_reflns_av_sigmaI/netI 0.0209
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_k_min -26
_diffrn_reflns_limit_k_max 25
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_theta_min 2.28
_diffrn_reflns_theta_max 39.12
_reflns_number_total 6281
_reflns_number_gt 5188
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2006)'
_computing_cell_refinement 'SAINT (Bruker, 2006)'
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact, 2006)'
_computing_publication_material ?
_publ_section_references
;
Bruker (2006). APEX2 (Version 2.1-0) and SAINT.
Bruker Analytical X-ray Systems, Madison, Wisconsin, USA.
Crystal Impact (2006). DIAMOND. Version3.1e. Crystal Impact GbR, Bonn,
Germany.
Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany.
Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of
G\"ottingen, Germany.
;
_publ_section_exptl_refinement
;
Hydrogen atoms for aromatic CH, aliphatic CH, CH~2~ and methyl groups
were positioned geometrically (C---H = 0.94 \%A for
aromatic CH, C---H = 0.99 \%A for aliphatic CH, C---H = 0.98 \%A for CH~2~,
C---H = 0.97 \%A for CH~3~) and refined using a
riding model (AFIX 43 for aromatic CH, AFIX 13 for aliphatic CH,
AFIX 23 for CH~2~, AFIX 33 or 137 for CH~3~),
with U~iso~(H) = 1.2U~eq~(CH) and U~iso~(H) = 1.5U~eq~(CH~3~).
;
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+0.7942P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 6281
_refine_ls_number_parameters 172
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0376
_refine_ls_R_factor_gt 0.0263
_refine_ls_wR_factor_ref 0.0719
_refine_ls_wR_factor_gt 0.0676
_refine_ls_goodness_of_fit_ref 1.024
_refine_ls_restrained_S_all 1.024
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
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
Zn Zn -0.765173(9) 0.190250(7) -0.376289(8) 0.01554(3) Uani 1 1 d . . .
O1 O -0.92606(6) 0.20951(5) -0.39044(7) 0.02245(13) Uani 1 1 d . . .
O2 O -1.02528(8) 0.10703(6) -0.52330(9) 0.0341(2) Uani 1 1 d . . .
O3 O -0.63969(8) 0.16719(6) -0.22099(7) 0.03092(18) Uani 1 1 d . . .
O4 O -0.71632(8) 0.03876(7) -0.29971(6) 0.03173(18) Uani 1 1 d . . .
N1 N -0.70190(7) 0.31711(5) -0.38139(7) 0.01728(13) Uani 1 1 d . . .
N2 N -0.71978(7) 0.36352(5) -0.47748(6) 0.01761(13) Uani 1 1 d . . .
N3 N -0.63097(7) 0.45066(5) -0.33156(6) 0.01686(13) Uani 1 1 d . . .
C1 C -0.67596(9) 0.44313(6) -0.44547(7) 0.01825(15) Uani 1 1 d . . .
H1 H -0.6758 0.4881 -0.4942 0.022 Uiso 1 1 calc R . .
C2 C -0.64827(9) 0.37074(6) -0.29478(8) 0.01879(15) Uani 1 1 d . . .
H2 H -0.6253 0.3561 -0.2187 0.023 Uiso 1 1 calc R . .
C3 C -0.56573(9) 0.52660(6) -0.26113(8) 0.01898(15) Uani 1 1 d . . .
H3A H -0.5688 0.5241 -0.1887 0.023 Uiso 1 1 calc R . .
H3B H -0.6050 0.5814 -0.2998 0.023 Uiso 1 1 calc R . .
C4 C -1.02269(8) 0.17156(7) -0.46525(8) 0.01958(15) Uani 1 1 d . . .
C5 C -1.14046(8) 0.21147(7) -0.48093(8) 0.01867(15) Uani 1 1 d . . .
C6 C -1.24912(9) 0.18091(7) -0.56897(9) 0.02154(17) Uani 1 1 d . . .
H6 H -1.2485 0.1343 -0.6154 0.026 Uiso 1 1 calc R . .
C7 C -1.35805(9) 0.21949(7) -0.58793(8) 0.02192(17) Uani 1 1 d . . .
H7 H -1.4310 0.1990 -0.6473 0.026 Uiso 1 1 calc R . .
C8 C -0.64558(9) 0.08295(7) -0.21666(8) 0.02233(18) Uani 1 1 d . . .
C9 C -0.56747(8) 0.03974(6) -0.10505(7) 0.01772(15) Uani 1 1 d . . .
C10 C -0.50011(9) 0.09112(6) -0.00969(8) 0.02128(17) Uani 1 1 d . . .
H10 H -0.4997 0.1528 -0.0164 0.026 Uiso 1 1 calc R . .
C11 C -0.43356(9) 0.05164(7) 0.09518(8) 0.02100(16) Uani 1 1 d . . .
H11 H -0.3891 0.0866 0.1597 0.025 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn 0.01517(5) 0.01693(5) 0.01218(5) 0.00254(3) 0.00430(4) 0.00080(3)
O1 0.0153(3) 0.0269(3) 0.0223(3) -0.0001(3) 0.0062(2) 0.0021(3)
O2 0.0220(3) 0.0322(4) 0.0428(5) -0.0130(4) 0.0104(3) 0.0030(3)
O3 0.0308(4) 0.0298(4) 0.0239(4) 0.0146(3) 0.0056(3) 0.0065(3)
O4 0.0252(3) 0.0464(5) 0.0143(3) 0.0057(3) 0.0012(3) 0.0013(3)
N1 0.0192(3) 0.0173(3) 0.0137(3) 0.0028(2) 0.0063(3) -0.0007(3)
N2 0.0222(3) 0.0160(3) 0.0139(3) 0.0026(2) 0.0077(3) 0.0003(3)
N3 0.0188(3) 0.0163(3) 0.0140(3) 0.0009(2) 0.0064(2) 0.0004(3)
C1 0.0227(4) 0.0159(3) 0.0149(3) 0.0022(3) 0.0076(3) 0.0012(3)
C2 0.0209(4) 0.0197(4) 0.0145(3) 0.0022(3) 0.0070(3) -0.0014(3)
C3 0.0205(4) 0.0158(3) 0.0191(4) -0.0025(3) 0.0078(3) 0.0000(3)
C4 0.0161(3) 0.0208(4) 0.0201(4) 0.0031(3) 0.0069(3) 0.0029(3)
C5 0.0153(3) 0.0215(4) 0.0174(3) 0.0023(3) 0.0059(3) 0.0020(3)
C6 0.0171(4) 0.0249(4) 0.0205(4) -0.0034(3) 0.0069(3) 0.0010(3)
C7 0.0155(3) 0.0273(5) 0.0193(4) -0.0030(3) 0.0049(3) 0.0002(3)
C8 0.0162(3) 0.0324(5) 0.0169(4) 0.0110(3) 0.0064(3) 0.0055(3)
C9 0.0151(3) 0.0205(4) 0.0137(3) 0.0047(3) 0.0033(3) 0.0018(3)
C10 0.0232(4) 0.0159(4) 0.0186(4) 0.0033(3) 0.0044(3) 0.0005(3)
C11 0.0207(4) 0.0200(4) 0.0149(3) 0.0004(3) 0.0018(3) -0.0013(3)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Zn O1 1.9465(7) . ?
Zn O3 1.9611(9) . ?
Zn N2 2.0328(8) 7_354 ?
Zn N1 2.0911(8) . ?
Zn O4 2.4712(10) . ?
Zn C8 2.5389(10) . ?
O1 C4 1.2901(12) . ?
O2 C4 1.2364(13) . ?
O3 C8 1.2818(14) . ?
O4 C8 1.2432(14) . ?
N1 C2 1.3120(12) . ?
N1 N2 1.3819(11) . ?
N2 C1 1.3119(12) . ?
N2 Zn 2.0328(8) 7_354 ?
N3 C1 1.3537(12) . ?
N3 C2 1.3598(12) . ?
N3 C3 1.4695(12) . ?
C1 H1 0.9400 . ?
C2 H2 0.9400 . ?
C3 C3 1.5240(19) 2_454 ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C4 C5 1.5097(13) . ?
C5 C7 1.3953(14) 7_254 ?
C5 C6 1.3981(14) . ?
C6 C7 1.3898(14) . ?
C6 H6 0.9400 . ?
C7 C5 1.3953(14) 7_254 ?
C7 H7 0.9400 . ?
C8 C9 1.4974(12) . ?
C9 C10 1.3907(13) . ?
C9 C11 1.3909(14) 5_455 ?
C10 C11 1.3855(13) . ?
C10 H10 0.9400 . ?
C11 C9 1.3909(14) 5_455 ?
C11 H11 0.9400 . ?
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
O1 Zn O3 114.50(4) . . ?
O1 Zn N2 109.27(3) . 7_354 ?
O3 Zn N2 127.62(4) . 7_354 ?
O1 Zn N1 104.21(3) . . ?
O3 Zn N1 93.91(4) . . ?
N2 Zn N1 102.01(3) 7_354 . ?
O1 Zn O4 103.09(3) . . ?
O3 Zn O4 58.40(3) . . ?
N2 Zn O4 85.24(3) 7_354 . ?
N1 Zn O4 147.44(3) . . ?
O1 Zn C8 111.02(3) . . ?
O3 Zn C8 29.71(4) . . ?
N2 Zn C8 107.49(4) 7_354 . ?
N1 Zn C8 122.09(3) . . ?
O4 Zn C8 28.69(3) . . ?
C4 O1 Zn 124.15(7) . . ?
C8 O3 Zn 100.97(7) . . ?
C8 O4 Zn 78.68(7) . . ?
C2 N1 N2 107.09(7) . . ?
C2 N1 Zn 126.07(6) . . ?
N2 N1 Zn 126.52(6) . . ?
C1 N2 N1 107.65(7) . . ?
C1 N2 Zn 121.31(6) . 7_354 ?
N1 N2 Zn 125.59(6) . 7_354 ?
C1 N3 C2 105.87(8) . . ?
C1 N3 C3 126.85(8) . . ?
C2 N3 C3 127.01(8) . . ?
N2 C1 N3 109.61(8) . . ?
N2 C1 H1 125.2 . . ?
N3 C1 H1 125.2 . . ?
N1 C2 N3 109.77(8) . . ?
N1 C2 H2 125.1 . . ?
N3 C2 H2 125.1 . . ?
N3 C3 C3 110.68(7) . 2_454 ?
N3 C3 H3A 109.5 . . ?
C3 C3 H3A 109.5 2_454 . ?
N3 C3 H3B 109.5 . . ?
C3 C3 H3B 109.5 2_454 . ?
H3A C3 H3B 108.1 . . ?
O2 C4 O1 125.42(9) . . ?
O2 C4 C5 119.10(9) . . ?
O1 C4 C5 115.48(9) . . ?
C7 C5 C6 119.75(9) 7_254 . ?
C7 C5 C4 121.03(9) 7_254 . ?
C6 C5 C4 119.17(9) . . ?
C7 C6 C5 120.02(9) . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C5 120.24(9) . 7_254 ?
C6 C7 H7 119.9 . . ?
C5 C7 H7 119.9 7_254 . ?
O4 C8 O3 121.93(9) . . ?
O4 C8 C9 120.91(10) . . ?
O3 C8 C9 117.10(9) . . ?
O4 C8 Zn 72.63(6) . . ?
O3 C8 Zn 49.31(5) . . ?
C9 C8 Zn 165.90(8) . . ?
C10 C9 C11 119.76(8) . 5_455 ?
C10 C9 C8 120.01(9) . . ?
C11 C9 C8 120.16(9) 5_455 . ?
C11 C10 C9 120.23(9) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C9 120.00(9) . 5_455 ?
C10 C11 H11 120.0 . . ?
C9 C11 H11 120.0 5_455 . ?
_diffrn_measured_fraction_theta_max 0.962
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max 0.614
_refine_diff_density_min -0.294
_refine_diff_density_rms 0.076
# Attachment '2.CIF'
data_m132_2
_database_code_depnum_ccdc_archive 'CCDC 695987'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
catena-[(\m4-benzene-1,4-dicarboxylato-\kO:\kO,O':\kO'':\kO'',O''')-
bis(\m4-1,2-bis(1,2,4-triazol-4-yl)ethane-\kN:\kN1':\kN2':\kN2')-
dicadmium(II) dinitrate hydrate]
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C10 H10 N6 O2 Cd, N O3, 0.5(O)'
_chemical_formula_sum 'C10 H10 Cd N7 O5.50'
_chemical_formula_weight 428.65
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'
Cd Cd -0.8075 1.2024 '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'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M C2/c
_symmetry_space_group_name_Hall '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 22.9206(8)
_cell_length_b 7.7047(2)
_cell_length_c 19.3208(7)
_cell_angle_alpha 90.00
_cell_angle_beta 114.596(3)
_cell_angle_gamma 90.00
_cell_volume 3102.40(18)
_cell_formula_units_Z 8
_cell_measurement_temperature 203(2)
_cell_measurement_reflns_used 6976
_cell_measurement_theta_min 2.318
_cell_measurement_theta_max 29.125
_exptl_crystal_description parallelepiped
_exptl_crystal_colour colorless
_exptl_crystal_size_max 0.32
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.02
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.835
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1688
_exptl_absorpt_coefficient_mu 1.448
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.6543
_exptl_absorpt_correction_T_max 0.9716
_exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 203(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker APEX2 CCD area detector'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 20459
_diffrn_reflns_av_R_equivalents 0.0395
_diffrn_reflns_av_sigmaI/netI 0.0227
_diffrn_reflns_limit_h_min -28
_diffrn_reflns_limit_h_max 28
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_theta_min 1.95
_diffrn_reflns_theta_max 25.85
_reflns_number_total 3001
_reflns_number_gt 2633
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2006)'
_computing_cell_refinement 'SAINT (Bruker, 2006)'
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact, 2006)'
_computing_publication_material ?
_publ_section_references
;
Bruker (2006). APEX2 (Version 2.1-0) and SAINT.
Bruker Analytical X-ray Systems, Madison, Wisconsin, USA.
Crystal Impact (2006). DIAMOND. Version3.1e. Crystal Impact GbR, Bonn,
Germany.
Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany.
Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of
G\"ottingen, Germany.
;
_publ_section_exptl_refinement
;
Hydrogen atoms for aromatic CH, aliphatic CH, CH~2~ and methyl groups
were positioned geometrically (C---H = 0.94 \%A for
aromatic CH, C---H = 0.99 \%A for aliphatic CH, C---H = 0.98 \%A for CH~2~,
C---H = 0.97 \%A for CH~3~) and refined using a
riding model (AFIX 43 for aromatic CH, AFIX 13 for aliphatic CH,
AFIX 23 for CH~2~, AFIX 33 or 137 for CH~3~),
with U~iso~(H) = 1.2U~eq~(CH) and U~iso~(H) = 1.5U~eq~(CH~3~).
The nitrate ions are disordered over at least two positions. Their N
and O atoms could only be refined isotropically.
The crystal water molecules have about 0.25 occupancy. Only the oxygen
atoms could be found and refined isotropically.
The maximum of the residual electron density is found within 1.1 \%A of the
cadmium atom.
;
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+10.1591P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 3001
_refine_ls_number_parameters 216
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0334
_refine_ls_R_factor_gt 0.0285
_refine_ls_wR_factor_ref 0.0774
_refine_ls_wR_factor_gt 0.0745
_refine_ls_goodness_of_fit_ref 1.053
_refine_ls_restrained_S_all 1.053
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
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
Cd Cd 0.247578(10) 0.28420(3) 0.272487(11) 0.01463(10) Uani 1 1 d . . .
O1 O 0.24950(12) 0.0801(3) 0.17776(12) 0.0267(5) Uani 1 1 d . . .
O2 O 0.25425(18) -0.1408(4) 0.11015(16) 0.0500(9) Uani 1 1 d . . .
C11 C 0.25129(17) 0.0180(5) 0.11836(18) 0.0238(7) Uani 1 1 d . . .
C12 C 0.25072(17) 0.1379(4) 0.05730(18) 0.0240(7) Uani 1 1 d . . .
C13 C 0.2487(2) 0.3175(5) 0.0652(2) 0.0319(9) Uani 1 1 d . . .
H13 H 0.2478 0.3638 0.1098 0.038 Uiso 1 1 calc R . .
C14 C 0.2520(2) 0.0716(5) -0.00875(19) 0.0329(9) Uani 1 1 d . . .
H14 H 0.2533 -0.0491 -0.0151 0.039 Uiso 1 1 calc R . .
N1 N 0.32783(13) 0.0910(4) 0.34824(15) 0.0248(6) Uani 1 1 d . . .
N2 N 0.33439(13) -0.0791(4) 0.33077(15) 0.0245(6) Uani 1 1 d . . .
C1 C 0.37493(19) 0.1246(5) 0.4136(2) 0.0387(9) Uani 1 1 d . . .
H1 H 0.3819 0.2317 0.4391 0.046 Uiso 1 1 calc R . .
C2 C 0.38510(17) -0.1412(5) 0.3865(2) 0.0355(9) Uani 1 1 d . . .
H2 H 0.4004 -0.2554 0.3894 0.043 Uiso 1 1 calc R . .
N3 N 0.41237(16) -0.0173(5) 0.43945(18) 0.0412(9) Uani 1 1 d . . .
C3 C 0.4725(2) -0.0298(7) 0.5091(2) 0.0537(13) Uani 1 1 d . . .
H3A H 0.4796 -0.1501 0.5273 0.064 Uiso 1 1 calc R . .
H3B H 0.4698 0.0432 0.5492 0.064 Uiso 1 1 calc R . .
N4 N 0.16821(13) 0.0852(4) 0.26511(18) 0.0269(6) Uani 1 1 d . . .
N5 N 0.16871(13) -0.0885(4) 0.24930(17) 0.0242(6) Uani 1 1 d . . .
C4 C 0.1198(2) 0.1116(6) 0.2823(3) 0.0465(11) Uani 1 1 d . . .
H4 H 0.1088 0.2194 0.2963 0.056 Uiso 1 1 calc R . .
C5 C 0.12038(17) -0.1584(5) 0.2575(2) 0.0335(9) Uani 1 1 d . . .
H5 H 0.1097 -0.2769 0.2505 0.040 Uiso 1 1 calc R . .
N6 N 0.08769(16) -0.0379(5) 0.2773(2) 0.0429(9) Uani 1 1 d . . .
C6 C 0.0284(2) -0.0595(7) 0.2885(3) 0.0569(14) Uani 1 1 d . . .
H6A H 0.0242 0.0356 0.3198 0.068 Uiso 1 1 calc R . .
H6B H 0.0299 -0.1691 0.3149 0.068 Uiso 1 1 calc R . .
N7 N 0.0065(5) 0.4503(12) 0.2735(4) 0.064(3) Uiso 0.50 1 d P A -1
O3 O -0.0296(7) 0.5039(18) 0.2924(8) 0.122(4) Uiso 0.50 1 d P A -1
O4A O 0.0090(8) 0.337(2) 0.3093(9) 0.070(4) Uiso 0.25 1 d P A -1
O4B O 0.0628(10) 0.492(3) 0.3197(13) 0.091(5) Uiso 0.25 1 d P A -1
O5 O 0.0512(7) 0.4974(19) 0.2660(10) 0.124(4) Uiso 0.50 1 d P A -1
N8 N -0.0085(7) 0.0207(18) 0.0265(8) 0.090(3) Uiso 0.50 1 d P B -2
O6 O 0.0327(6) -0.0367(16) 0.0721(7) 0.108(3) Uiso 0.50 1 d P B -2
O7 O -0.0251(8) 0.140(3) 0.0540(9) 0.159(5) Uiso 0.50 1 d P B -2
O8 O -0.0441(9) 0.000(2) -0.0317(12) 0.164(6) Uiso 0.50 1 d P B -2
O10 O 0.0876(16) 0.037(4) -0.0229(18) 0.168(12) Uiso 0.25 1 d P C -2
O9 O 0.1297(10) 0.252(2) 0.4305(11) 0.088(5) Uiso 0.25 1 d P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd 0.01741(14) 0.01203(15) 0.01525(13) -0.00031(8) 0.00761(10) 0.00003(8)
O1 0.0455(14) 0.0211(13) 0.0200(11) 0.0013(10) 0.0203(11) -0.0009(11)
O2 0.115(3) 0.0157(14) 0.0369(15) 0.0035(12) 0.0490(18) 0.0019(16)
C11 0.0325(18) 0.0227(19) 0.0177(15) 0.0028(14) 0.0120(14) 0.0002(15)
C12 0.0380(19) 0.0165(18) 0.0218(16) 0.0020(14) 0.0168(15) 0.0006(15)
C13 0.059(2) 0.023(2) 0.0219(17) -0.0003(15) 0.0247(17) 0.0021(17)
C14 0.062(3) 0.0163(17) 0.0267(18) 0.0021(15) 0.0254(18) 0.0013(17)
N1 0.0248(14) 0.0176(15) 0.0222(13) -0.0014(11) 0.0001(11) -0.0006(12)
N2 0.0218(13) 0.0197(15) 0.0240(14) 0.0005(12) 0.0016(11) 0.0001(12)
C1 0.037(2) 0.027(2) 0.0323(19) -0.0039(17) -0.0050(16) -0.0016(17)
C2 0.0265(18) 0.028(2) 0.036(2) 0.0003(17) -0.0033(16) 0.0054(16)
N3 0.0313(17) 0.036(2) 0.0305(16) 0.0017(15) -0.0125(14) 0.0024(15)
C3 0.037(2) 0.056(3) 0.035(2) 0.003(2) -0.0191(19) 0.002(2)
N4 0.0246(14) 0.0148(14) 0.0494(18) -0.0017(13) 0.0236(13) -0.0016(12)
N5 0.0209(13) 0.0172(15) 0.0399(16) -0.0028(12) 0.0179(12) -0.0003(12)
C4 0.043(2) 0.027(2) 0.090(3) 0.000(2) 0.048(2) 0.0044(18)
C5 0.0277(18) 0.0245(19) 0.056(2) -0.0060(18) 0.0250(18) -0.0063(16)
N6 0.0294(17) 0.034(2) 0.085(3) -0.0012(19) 0.0433(18) -0.0027(15)
C6 0.040(2) 0.050(3) 0.108(4) -0.006(3) 0.058(3) -0.007(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Cd N4 2.338(3) . ?
Cd N5 2.344(3) 4 ?
Cd N2 2.345(3) 4 ?
Cd N1 2.345(3) . ?
Cd O2 2.357(2) 4 ?
Cd O1 2.427(2) . ?
Cd O1 2.464(2) 4 ?
O1 C11 1.260(4) . ?
O1 Cd 2.464(2) 4_545 ?
O2 C11 1.239(4) . ?
O2 Cd 2.357(2) 4_545 ?
C11 C12 1.494(4) . ?
C12 C14 1.386(5) . ?
C12 C13 1.395(5) . ?
C13 C14 1.381(5) 7 ?
C13 H13 0.9400 . ?
C14 C13 1.381(5) 7 ?
C14 H14 0.9400 . ?
N1 C1 1.301(4) . ?
N1 N2 1.377(4) . ?
N2 C2 1.303(4) . ?
N2 Cd 2.345(3) 4_545 ?
C1 N3 1.350(5) . ?
C1 H1 0.9400 . ?
C2 N3 1.348(5) . ?
C2 H2 0.9400 . ?
N3 C3 1.475(5) . ?
C3 C3 1.514(10) 5_656 ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
N4 C4 1.300(5) . ?
N4 N5 1.374(4) . ?
N5 C5 1.299(4) . ?
N5 Cd 2.344(3) 4_545 ?
C4 N6 1.349(6) . ?
C4 H4 0.9400 . ?
C5 N6 1.345(5) . ?
C5 H5 0.9400 . ?
N6 C6 1.472(4) . ?
C6 C6 1.514(11) 2 ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
N7 O4A 1.097(17) . ?
N7 O3 1.113(14) . ?
N7 O5 1.150(16) . ?
N7 O4B 1.27(2) . ?
O3 O4A 1.51(2) . ?
O4A O4B 1.67(3) . ?
O4B O5 0.959(19) . ?
N8 O6 1.082(16) . ?
N8 O8 1.091(18) . ?
N8 O7 1.201(19) . ?
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
N4 Cd N5 159.72(10) . 4 ?
N4 Cd N2 85.13(10) . 4 ?
N5 Cd N2 94.89(10) 4 4 ?
N4 Cd N1 90.58(10) . . ?
N5 Cd N1 83.66(10) 4 . ?
N2 Cd N1 163.44(10) 4 . ?
N4 Cd O2 83.95(11) . 4 ?
N5 Cd O2 114.44(11) 4 4 ?
N2 Cd O2 112.31(11) 4 4 ?
N1 Cd O2 83.03(11) . 4 ?
N4 Cd O1 77.70(9) . . ?
N5 Cd O1 82.10(9) 4 . ?
N2 Cd O1 84.78(9) 4 . ?
N1 Cd O1 78.68(9) . . ?
O2 Cd O1 153.81(9) 4 . ?
N4 Cd O1 121.65(9) . 4 ?
N5 Cd O1 77.97(9) 4 4 ?
N2 Cd O1 78.38(9) 4 4 ?
N1 Cd O1 117.18(9) . 4 ?
O2 Cd O1 53.58(9) 4 4 ?
O1 Cd O1 152.56(7) . 4 ?
C11 O1 Cd 161.9(2) . . ?
C11 O1 Cd 89.9(2) . 4_545 ?
Cd O1 Cd 108.14(8) . 4_545 ?
C11 O2 Cd 95.5(2) . 4_545 ?
O2 C11 O1 121.1(3) . . ?
O2 C11 C12 119.5(3) . . ?
O1 C11 C12 119.4(3) . . ?
C14 C12 C13 118.8(3) . . ?
C14 C12 C11 120.1(3) . . ?
C13 C12 C11 121.1(3) . . ?
C14 C13 C12 121.1(3) 7 . ?
C14 C13 H13 119.4 7 . ?
C12 C13 H13 119.4 . . ?
C13 C14 C12 120.1(3) 7 . ?
C13 C14 H14 119.9 7 . ?
C12 C14 H14 119.9 . . ?
C1 N1 N2 107.2(3) . . ?
C1 N1 Cd 126.7(3) . . ?
N2 N1 Cd 126.05(19) . . ?
C2 N2 N1 107.3(3) . . ?
C2 N2 Cd 131.4(3) . 4_545 ?
N1 N2 Cd 120.35(19) . 4_545 ?
N1 C1 N3 109.9(3) . . ?
N1 C1 H1 125.0 . . ?
N3 C1 H1 125.0 . . ?
N2 C2 N3 109.8(3) . . ?
N2 C2 H2 125.1 . . ?
N3 C2 H2 125.1 . . ?
C2 N3 C1 105.7(3) . . ?
C2 N3 C3 127.4(4) . . ?
C1 N3 C3 126.8(4) . . ?
N3 C3 C3 108.7(4) . 5_656 ?
N3 C3 H3A 110.0 . . ?
C3 C3 H3A 110.0 5_656 . ?
N3 C3 H3B 110.0 . . ?
C3 C3 H3B 110.0 5_656 . ?
H3A C3 H3B 108.3 . . ?
C4 N4 N5 107.2(3) . . ?
C4 N4 Cd 127.4(3) . . ?
N5 N4 Cd 125.05(19) . . ?
C5 N5 N4 106.9(3) . . ?
C5 N5 Cd 130.7(3) . 4_545 ?
N4 N5 Cd 122.05(19) . 4_545 ?
N4 C4 N6 110.3(4) . . ?
N4 C4 H4 124.9 . . ?
N6 C4 H4 124.9 . . ?
N5 C5 N6 110.7(3) . . ?
N5 C5 H5 124.7 . . ?
N6 C5 H5 124.7 . . ?
C5 N6 C4 104.9(3) . . ?
C5 N6 C6 128.4(4) . . ?
C4 N6 C6 126.6(4) . . ?
N6 C6 C6 109.0(5) . 2 ?
N6 C6 H6A 109.9 . . ?
C6 C6 H6A 109.9 2 . ?
N6 C6 H6B 109.9 . . ?
C6 C6 H6B 109.9 2 . ?
H6A C6 H6B 108.3 . . ?
O4A N7 O3 86.5(13) . . ?
O4A N7 O5 120.8(16) . . ?
O3 N7 O5 138.2(13) . . ?
O4A N7 O4B 89.2(15) . . ?
O3 N7 O4B 110.5(13) . . ?
O5 N7 O4B 46.4(10) . . ?
N7 O3 O4A 46.3(9) . . ?
N7 O4A O3 47.2(10) . . ?
N7 O4A O4B 49.6(12) . . ?
O3 O4A O4B 75.9(12) . . ?
O5 O4B N7 60.3(15) . . ?
O5 O4B O4A 92(2) . . ?
N7 O4B O4A 41.2(9) . . ?
O4B O5 N7 73.3(16) . . ?
O6 N8 O8 144(2) . . ?
O6 N8 O7 106.4(16) . . ?
O8 N8 O7 109(2) . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 25.85
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 1.581
_refine_diff_density_min -0.589
_refine_diff_density_rms 0.100
# Attachment '3.CIF'
data_m212
_database_code_depnum_ccdc_archive 'CCDC 695988'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
catena-[diaqua-bis(\m3-benzene-1,3-dicarboxylato-\kO:\kO':\kO'')-
(\m2-1,2-bis(1,2,4-triazol-4-yl)ethane-\kN1:\kN1')-dizinc(II)] dihydrate
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C11 H12 N3 O5 Zn, H2 O'
_chemical_formula_sum 'C11 H12 N3 O6 Zn'
_chemical_formula_weight 347.63
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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Triclinic
_symmetry_space_group_name_H-M P-1
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 7.4247(2)
_cell_length_b 9.3631(2)
_cell_length_c 10.1580(2)
_cell_angle_alpha 81.6570(10)
_cell_angle_beta 70.6750(10)
_cell_angle_gamma 71.7040(10)
_cell_volume 632.02(3)
_cell_formula_units_Z 2
_cell_measurement_temperature 203(2)
_cell_measurement_reflns_used 3968
_cell_measurement_theta_min 3.03
_cell_measurement_theta_max 35.5
_exptl_crystal_description parallelepiped
_exptl_crystal_colour colorless
_exptl_crystal_size_max 0.25
_exptl_crystal_size_mid 0.09
_exptl_crystal_size_min 0.01
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.827
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 354
_exptl_absorpt_coefficient_mu 1.977
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.6378
_exptl_absorpt_correction_T_max 0.9805
_exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 203(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker APEX2 CCD area detector'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 8293
_diffrn_reflns_av_R_equivalents 0.0192
_diffrn_reflns_av_sigmaI/netI 0.0312
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_theta_min 2.13
_diffrn_reflns_theta_max 35.63
_reflns_number_total 4087
_reflns_number_gt 3464
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2006)'
_computing_cell_refinement 'SAINT (Bruker, 2006)'
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact, 2006)'
_computing_publication_material ?
_publ_section_references
;
Bruker (2006). APEX2 (Version 2.1-0) and SAINT.
Bruker Analytical X-ray Systems, Madison, Wisconsin, USA.
Crystal Impact (2006). DIAMOND. Version3.1e. Crystal Impact GbR, Bonn,
Germany.
Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany.
Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of
G\"ottingen, Germany.
;
_publ_section_exptl_refinement
;
Hydrogen atoms for aromatic CH, aliphatic CH, CH~2~ and methyl groups
were positioned geometrically (C---H = 0.94 \%A for
aromatic CH, C---H = 0.99 \%A for aliphatic CH, C---H = 0.98 \%A for CH~2~,
C---H = 0.97 \%A for CH~3~) and refined using a
riding model (AFIX 43 for aromatic CH, AFIX 13 for aliphatic CH,
AFIX 23 for CH~2~, AFIX 33 or 137 for CH~3~),
with U~iso~(H) = 1.2U~eq~(CH) and U~iso~(H) = 1.5U~eq~(CH~3~).
Hydrogen atoms of the aqua ligand and the water molecule of
crystallization were found and refined with U~iso~(H) = 1.5U~eq~(O).
;
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+0.2037P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 4087
_refine_ls_number_parameters 202
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0394
_refine_ls_R_factor_gt 0.0304
_refine_ls_wR_factor_ref 0.0741
_refine_ls_wR_factor_gt 0.0702
_refine_ls_goodness_of_fit_ref 1.038
_refine_ls_restrained_S_all 1.038
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
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
Zn Zn 0.00765(3) 0.741199(19) 0.446532(19) 0.01720(7) Uani 1 1 d . . .
N1 N -0.0048(2) 0.73799(15) 0.65464(15) 0.0183(3) Uani 1 1 d . . .
N2 N -0.1290(2) 0.84954(15) 0.74623(16) 0.0212(3) Uani 1 1 d . . .
N3 N 0.0090(2) 0.65483(15) 0.86331(15) 0.0184(3) Uani 1 1 d . . .
C1 C 0.0760(3) 0.62312(18) 0.72756(18) 0.0197(3) Uani 1 1 d . . .
H1 H 0.1670 0.5324 0.6905 0.024 Uiso 1 1 calc R . .
C2 C -0.1190(3) 0.79561(18) 0.86982(18) 0.0214(4) Uani 1 1 d . . .
H2 H -0.1909 0.8472 0.9526 0.026 Uiso 1 1 calc R . .
C3 C 0.0601(3) 0.55608(18) 0.97902(18) 0.0199(3) Uani 1 1 d . . .
H3A H 0.0314 0.6162 1.0587 0.024 Uiso 1 1 calc R . .
H3B H 0.2025 0.5026 0.9504 0.024 Uiso 1 1 calc R . .
O1 O 0.22694(18) 0.57517(13) 0.34322(14) 0.0246(3) Uani 1 1 d . . .
O2 O 0.19506(17) 0.39224(13) 0.50984(13) 0.0196(2) Uani 1 1 d . . .
O3 O 0.80709(19) -0.06258(13) 0.42045(14) 0.0246(3) Uani 1 1 d . . .
O4 O 0.9139(2) -0.15428(15) 0.21150(17) 0.0395(4) Uani 1 1 d . . .
C11 C 0.4321(2) 0.32965(16) 0.28733(17) 0.0157(3) Uani 1 1 d . . .
C12 C 0.5394(2) 0.19454(17) 0.33705(17) 0.0160(3) Uani 1 1 d . . .
H12 H 0.5128 0.1726 0.4337 0.019 Uiso 1 1 calc R . .
C13 C 0.6866(2) 0.09156(17) 0.24291(18) 0.0169(3) Uani 1 1 d . . .
C14 C 0.7196(3) 0.12377(19) 0.10000(18) 0.0207(3) Uani 1 1 d . . .
H14 H 0.8171 0.0541 0.0364 0.025 Uiso 1 1 calc R . .
C15 C 0.6110(3) 0.25661(19) 0.05066(18) 0.0215(4) Uani 1 1 d . . .
H15 H 0.6328 0.2766 -0.0459 0.026 Uiso 1 1 calc R . .
C16 C 0.4689(2) 0.36078(18) 0.14506(18) 0.0189(3) Uani 1 1 d . . .
H16 H 0.3975 0.4528 0.1119 0.023 Uiso 1 1 calc R . .
C17 C 0.2724(2) 0.43974(17) 0.38897(18) 0.0177(3) Uani 1 1 d . . .
C18 C 0.8111(2) -0.05173(18) 0.2929(2) 0.0216(4) Uani 1 1 d . . .
O5 O 0.23105(19) 0.86589(14) 0.38831(15) 0.0236(3) Uani 1 1 d . . .
H5A H 0.212(4) 0.935(3) 0.336(3) 0.035 Uiso 1 1 d . . .
H5B H 0.216(4) 0.907(3) 0.459(3) 0.035 Uiso 1 1 d . . .
O6 O 0.6203(3) 0.6920(2) 0.2117(2) 0.0512(5) Uani 1 1 d . . .
H6A H 0.499(5) 0.721(4) 0.278(4) 0.077 Uiso 1 1 d . . .
H6B H 0.685(5) 0.750(4) 0.239(3) 0.077 Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn 0.01839(10) 0.01126(9) 0.01584(11) 0.00126(7) -0.00419(7) 0.00220(6)
N1 0.0211(7) 0.0165(6) 0.0157(7) 0.0034(5) -0.0064(5) -0.0042(5)
N2 0.0268(7) 0.0139(6) 0.0207(7) 0.0022(5) -0.0069(6) -0.0044(5)
N3 0.0255(7) 0.0148(6) 0.0154(7) 0.0036(5) -0.0076(6) -0.0068(5)
C1 0.0229(8) 0.0180(7) 0.0162(8) 0.0012(6) -0.0068(6) -0.0031(6)
C2 0.0282(9) 0.0157(7) 0.0188(8) -0.0002(6) -0.0060(7) -0.0056(6)
C3 0.0277(8) 0.0188(7) 0.0160(8) 0.0043(6) -0.0107(7) -0.0085(6)
O1 0.0215(6) 0.0101(5) 0.0298(7) 0.0020(5) 0.0019(5) 0.0009(4)
O2 0.0195(5) 0.0166(5) 0.0184(6) -0.0011(5) -0.0031(5) -0.0020(4)
O3 0.0251(6) 0.0150(5) 0.0315(8) 0.0082(5) -0.0133(6) -0.0018(5)
O4 0.0361(8) 0.0172(6) 0.0452(10) -0.0042(6) -0.0005(7) 0.0087(6)
C11 0.0134(6) 0.0116(6) 0.0202(8) 0.0000(6) -0.0054(6) -0.0011(5)
C12 0.0145(7) 0.0134(6) 0.0175(8) 0.0000(6) -0.0047(6) -0.0008(5)
C13 0.0153(7) 0.0116(6) 0.0209(8) 0.0007(6) -0.0047(6) -0.0015(5)
C14 0.0199(7) 0.0183(7) 0.0204(8) -0.0052(6) -0.0032(6) -0.0017(6)
C15 0.0243(8) 0.0223(8) 0.0168(8) 0.0006(7) -0.0068(7) -0.0054(6)
C16 0.0183(7) 0.0152(7) 0.0206(8) 0.0039(6) -0.0067(6) -0.0022(6)
C17 0.0147(7) 0.0124(6) 0.0245(9) -0.0031(6) -0.0067(6) -0.0002(5)
C18 0.0164(7) 0.0121(7) 0.0314(10) 0.0040(7) -0.0052(7) -0.0017(6)
O5 0.0255(6) 0.0149(5) 0.0268(7) 0.0033(5) -0.0072(5) -0.0033(5)
O6 0.0316(8) 0.0611(12) 0.0523(11) -0.0237(9) -0.0084(8) 0.0031(8)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Zn O1 1.9805(11) . ?
Zn O3 2.0162(11) 1_465 ?
Zn N1 2.0814(14) . ?
Zn O2 2.1450(13) 2_566 ?
Zn O5 2.1978(14) . ?
N1 C1 1.313(2) . ?
N1 N2 1.3843(19) . ?
N2 C2 1.300(2) . ?
N3 C1 1.345(2) . ?
N3 C2 1.357(2) . ?
N3 C3 1.463(2) . ?
C1 H1 0.9400 . ?
C2 H2 0.9400 . ?
C3 C3 1.512(4) 2_567 ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
O1 C17 1.2656(19) . ?
O2 C17 1.253(2) . ?
O2 Zn 2.1450(13) 2_566 ?
O3 C18 1.276(2) . ?
O3 Zn 2.0162(11) 1_645 ?
O4 C18 1.241(2) . ?
C11 C16 1.384(2) . ?
C11 C12 1.392(2) . ?
C11 C17 1.505(2) . ?
C12 C13 1.397(2) . ?
C12 H12 0.9400 . ?
C13 C14 1.394(2) . ?
C13 C18 1.499(2) . ?
C14 C15 1.380(2) . ?
C14 H14 0.9400 . ?
C15 C16 1.393(2) . ?
C15 H15 0.9400 . ?
C16 H16 0.9400 . ?
O5 H5A 0.79(3) . ?
O5 H5B 0.82(2) . ?
O6 H6A 0.91(4) . ?
O6 H6B 0.95(3) . ?
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
O1 Zn O3 142.84(6) . 1_465 ?
O1 Zn N1 112.75(5) . . ?
O3 Zn N1 103.59(5) 1_465 . ?
O1 Zn O2 90.35(5) . 2_566 ?
O3 Zn O2 94.99(5) 1_465 2_566 ?
N1 Zn O2 93.69(5) . 2_566 ?
O1 Zn O5 85.33(5) . . ?
O3 Zn O5 87.59(5) 1_465 . ?
N1 Zn O5 89.37(6) . . ?
O2 Zn O5 175.42(4) 2_566 . ?
C1 N1 N2 107.73(13) . . ?
C1 N1 Zn 126.68(11) . . ?
N2 N1 Zn 124.74(10) . . ?
C2 N2 N1 106.28(13) . . ?
C1 N3 C2 105.34(14) . . ?
C1 N3 C3 126.94(14) . . ?
C2 N3 C3 127.70(14) . . ?
N1 C1 N3 109.73(14) . . ?
N1 C1 H1 125.1 . . ?
N3 C1 H1 125.1 . . ?
N2 C2 N3 110.90(14) . . ?
N2 C2 H2 124.5 . . ?
N3 C2 H2 124.5 . . ?
N3 C3 C3 109.49(16) . 2_567 ?
N3 C3 H3A 109.8 . . ?
C3 C3 H3A 109.8 2_567 . ?
N3 C3 H3B 109.8 . . ?
C3 C3 H3B 109.8 2_567 . ?
H3A C3 H3B 108.2 . . ?
C17 O1 Zn 125.10(12) . . ?
C17 O2 Zn 122.70(10) . 2_566 ?
C18 O3 Zn 106.76(10) . 1_645 ?
C16 C11 C12 120.08(14) . . ?
C16 C11 C17 120.19(13) . . ?
C12 C11 C17 119.71(15) . . ?
C11 C12 C13 119.83(15) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C14 C13 C12 119.31(14) . . ?
C14 C13 C18 119.50(14) . . ?
C12 C13 C18 121.19(15) . . ?
C15 C14 C13 120.88(14) . . ?
C15 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
C14 C15 C16 119.46(16) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 H15 120.3 . . ?
C11 C16 C15 120.40(14) . . ?
C11 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
O2 C17 O1 125.25(14) . . ?
O2 C17 C11 118.80(14) . . ?
O1 C17 C11 115.94(15) . . ?
O4 C18 O3 122.22(16) . . ?
O4 C18 C13 120.34(17) . . ?
O3 C18 C13 117.44(14) . . ?
Zn O5 H5A 114.8(18) . . ?
Zn O5 H5B 106.4(18) . . ?
H5A O5 H5B 101(2) . . ?
H6A O6 H6B 98(3) . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5A N2 0.79(3) 2.05(3) 2.8110(19) 163(2) 2_576
O5 H5B O3 0.82(2) 1.97(2) 2.7555(18) 161(2) 2_666
O6 H6A O5 0.91(4) 2.08(4) 2.947(2) 157(3) .
O6 H6B O4 0.95(3) 2.09(4) 2.965(3) 154(3) 1_565
_diffrn_measured_fraction_theta_max 0.701
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.968
_refine_diff_density_max 0.472
_refine_diff_density_min -0.335
_refine_diff_density_rms 0.075