data_2203293
loop_
_publ_author_name
'Liang Shen'
' Mei Chao Li '
' Zhi Min Jin '
' Mao Lin Hu '
' Ri Cheng Xuan '
_publ_section_title
;
Bis[(3-amino-5-methyl-isoxazole)-N-]zinc(II)dichloride
;
_journal_issue                 3
_journal_name_full             'Acta Crystallographica, Section E'
_journal_page_first            m330
_journal_page_last             m331
_journal_volume                60
_journal_year                  2004
_chemical_formula_iupac        '[Zn (C4 H6 N2 O )2 Cl2]'
_chemical_formula_moiety       'C8 H12 Cl2 N4 O2 Zn'
_chemical_formula_sum          'C8 H12 Cl2 N4 O2 Zn'
_chemical_formula_weight       332.49
_chemical_melting_point        ?
_chemical_name_common          ?
_chemical_name_systematic
;
bis[(3-Amino-5-methyl-isoxazole)-N-]zinc(II)dichloride
;
_symmetry_cell_setting         Orthorhombic
_symmetry_space_group_name_Hall '-P 2ab 2ac'
_symmetry_space_group_name_H-M 'Pccn '
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary   direct
_atom_sites_solution_secondary difmap
_audit_creation_method         SHELXL-97
_cell_angle_alpha              90.0
_cell_angle_beta               90.0
_cell_angle_gamma              90.0
_cell_formula_units_Z          8
_cell_length_a                 13.105(3)
_cell_length_b                 14.054(3)
_cell_length_c                 14.344(3)
_cell_measurement_reflns_used  596
_cell_measurement_temperature  293(2)
_cell_measurement_theta_max    22.42
_cell_measurement_theta_min    2.55
_cell_volume                   2641.8(10)
_computing_cell_refinement     ' SMART '
_computing_data_collection     ' SMART (Bruker, 2000) '
_computing_data_reduction      ' SAINT (Bruker, 2000) '
_computing_molecular_graphics  ' SHELXTL '
_computing_publication_material ' SHELXTL '
_computing_structure_refinement ' SHELXTL '
_computing_structure_solution  ' SHELXTL (Bruker, 2000) '
_diffrn_ambient_temperature    293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type 'Bruker SMART CCD area-detector'
_diffrn_measurement_method     '\f and \w 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 0.0286
_diffrn_reflns_av_sigmaI/netI  0.0363
_diffrn_reflns_limit_h_max     16
_diffrn_reflns_limit_h_min     -13
_diffrn_reflns_limit_k_max     17
_diffrn_reflns_limit_k_min     -16
_diffrn_reflns_limit_l_max     17
_diffrn_reflns_limit_l_min     -17
_diffrn_reflns_number          13278
_diffrn_reflns_theta_full      25.99
_diffrn_reflns_theta_max       25.99
_diffrn_reflns_theta_min       2.12
_diffrn_standards_decay_%      0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_number       0
_exptl_absorpt_coefficient_mu  2.259
_exptl_absorpt_correction_T_max 0.71
_exptl_absorpt_correction_T_min 0.67
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details '(SADABS; Bruker, 2000)'
_exptl_crystal_colour          colorless
_exptl_crystal_density_diffrn  1.672
_exptl_crystal_density_meas    ?
_exptl_crystal_density_method  'not measured'
_exptl_crystal_description     prism
_exptl_crystal_F_000           1344
_exptl_crystal_size_max        0.25
_exptl_crystal_size_mid        0.15
_exptl_crystal_size_min        0.15
_refine_diff_density_max       0.494
_refine_diff_density_min       -0.526
_refine_ls_extinction_coef     ?
_refine_ls_extinction_method   none
_refine_ls_goodness_of_fit_ref 1.240
_refine_ls_hydrogen_treatment  constr
_refine_ls_matrix_type         full
_refine_ls_number_parameters   156
_refine_ls_number_reflns       2602
_refine_ls_number_restraints   0
_refine_ls_restrained_S_all    1.240
_refine_ls_R_factor_all        0.0834
_refine_ls_R_factor_gt         0.0568
_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/[\s^2^(Fo^2^)+(0.0752P)^2^+0.0000P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme    calc
_refine_ls_wR_factor_gt        0.1503
_refine_ls_wR_factor_ref       0.1548
_reflns_number_gt              1744
_reflns_number_total           2602
_reflns_threshold_expression   >2\s(I)
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Zn 0.12762(4) 1.00532(3) 0.22473(4) 0.0443(2) Uani d . 1 . . Zn
Cl1 0.12265(10) 0.87644(9) 0.31617(10) 0.0582(4) Uani d . 1 . . Cl
Cl2 0.13508(10) 1.15091(8) 0.28695(10) 0.0592(4) Uani d . 1 . . Cl
C1 -0.0825(4) 1.0538(3) 0.1362(3) 0.0409(10) Uani d . 1 . . C
C2 -0.1553(4) 1.0027(3) 0.0853(4) 0.0506(12) Uani d . 1 . . C
H2 -0.2211 1.0222 0.0705 0.061 Uiso calc R 1 . . H
C3 -0.1112(3) 0.9206(3) 0.0624(3) 0.0422(9) Uani d . 1 . . C
C4 -0.1459(4) 0.8356(4) 0.0097(4) 0.0651(15) Uani d . 1 . . C
H4A -0.1428 0.7806 0.0493 0.098 Uiso calc R 1 . . H
H4B -0.1025 0.8261 -0.0434 0.098 Uiso calc R 1 . . H
H4C -0.2149 0.8451 -0.0109 0.098 Uiso calc R 1 . . H
C5 0.3442(4) 1.0323(3) 0.1422(3) 0.0393(10) Uani d . 1 . . C
C6 0.4160(4) 0.9715(3) 0.1018(3) 0.0454(11) Uani d . 1 . . C
H6 0.4834 0.9855 0.0869 0.054 Uiso calc R 1 . . H
C7 0.3679(3) 0.8895(3) 0.0892(3) 0.0463(11) Uani d . 1 . . C
C8 0.3991(5) 0.7943(4) 0.0547(4) 0.0699(15) Uani d . 1 . . C
H8A 0.4717 0.7932 0.0455 0.105 Uiso calc R 1 . . H
H8B 0.3654 0.7813 -0.0033 0.105 Uiso calc R 1 . . H
H8C 0.3805 0.7468 0.0997 0.105 Uiso calc R 1 . . H
N1 0.0014(3) 1.0034(2) 0.1452(3) 0.0467(9) Uani d . 1 . . N
N2 -0.0914(4) 1.1408(3) 0.1727(3) 0.0684(13) Uani d . 1 . . N
H2A -0.0414 1.1653 0.2031 0.082 Uiso calc R 1 . . H
H2B -0.1472 1.1722 0.1658 0.082 Uiso calc R 1 . . H
N3 0.2558(3) 0.9902(2) 0.1503(3) 0.0448(9) Uani d . 1 . . N
N4 0.3590(3) 1.1232(3) 0.1690(3) 0.0552(12) Uani d . 1 . . N
H4E 0.3090 1.1566 0.1899 0.066 Uiso d R 1 . . H
H4D 0.4183 1.1485 0.1628 0.066 Uiso d R 1 . . H
O1 -0.0164(2) 0.9168(2) 0.0972(2) 0.0491(8) Uani d . 1 . . O
O2 0.2697(2) 0.89698(19) 0.1159(2) 0.0495(8) Uani d . 1 . . O
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Zn 0.0346(3) 0.0334(3) 0.0648(4) -0.0019(2) 0.0026(2) -0.0030(2)
Cl1 0.0499(7) 0.0426(6) 0.0822(9) -0.0025(5) -0.0005(6) 0.0127(6)
Cl2 0.0568(8) 0.0387(6) 0.0823(9) -0.0053(5) 0.0112(6) -0.0151(6)
C1 0.041(3) 0.038(2) 0.044(2) 0.0054(18) 0.0060(19) 0.0112(19)
C2 0.034(2) 0.064(3) 0.055(3) 0.023(2) -0.004(2) 0.016(2)
C3 0.035(2) 0.045(2) 0.047(2) 0.0004(19) -0.0088(18) 0.0105(19)
C4 0.061(3) 0.052(3) 0.083(4) -0.017(2) -0.029(3) 0.008(3)
C5 0.039(2) 0.036(2) 0.043(2) 0.0004(18) -0.0079(18) 0.0019(18)
C6 0.038(2) 0.052(3) 0.046(2) 0.005(2) 0.014(2) 0.009(2)
C7 0.045(3) 0.050(3) 0.044(2) 0.007(2) 0.0034(19) 0.001(2)
C8 0.076(4) 0.055(3) 0.078(4) 0.017(3) 0.007(3) -0.011(3)
N1 0.0335(19) 0.0368(17) 0.070(3) 0.0047(15) -0.0036(18) -0.0049(17)
N2 0.077(3) 0.041(2) 0.087(3) 0.030(2) -0.009(3) -0.008(2)
N3 0.035(2) 0.0362(17) 0.063(2) 0.0085(16) 0.0021(17) -0.0085(16)
N4 0.029(2) 0.0402(19) 0.097(3) -0.0072(16) 0.0046(19) 0.005(2)
O1 0.0307(16) 0.0378(15) 0.079(2) 0.0043(13) -0.0107(14) -0.0108(15)
O2 0.0386(16) 0.0415(16) 0.068(2) 0.0002(14) -0.0012(15) -0.0058(14)
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'
Cl Cl 0.1484 0.1585 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N3 Zn N1 . . 112.74(18) ?
N3 Zn Cl2 . . 105.87(11) ?
N1 Zn Cl2 . . 105.96(10) ?
N3 Zn Cl1 . . 104.55(11) ?
N1 Zn Cl1 . . 107.35(11) ?
Cl2 Zn Cl1 . . 120.56(6) ?
N1 C1 N2 . . 121.8(5) ?
N1 C1 C2 . . 110.2(4) ?
N2 C1 C2 . . 127.9(5) ?
C3 C2 C1 . . 106.1(4) ?
C3 C2 H2 . . 126.9 ?
C1 C2 H2 . . 126.9 ?
C2 C3 O1 . . 110.1(4) ?
C2 C3 C4 . . 133.6(4) ?
O1 C3 C4 . . 116.2(4) ?
C3 C4 H4A . . 109.5 ?
C3 C4 H4B . . 109.5 ?
H4A C4 H4B . . 109.5 ?
C3 C4 H4C . . 109.5 ?
H4A C4 H4C . . 109.5 ?
H4B C4 H4C . . 109.5 ?
N3 C5 N4 . . 122.1(4) ?
N3 C5 C6 . . 110.9(4) ?
N4 C5 C6 . . 127.0(5) ?
C7 C6 C5 . . 105.6(4) ?
C7 C6 H6 . . 127.2 ?
C5 C6 H6 . . 127.2 ?
C6 C7 O2 . . 110.3(4) ?
C6 C7 C8 . . 134.3(5) ?
O2 C7 C8 . . 115.4(4) ?
C7 C8 H8A . . 109.5 ?
C7 C8 H8B . . 109.5 ?
H8A C8 H8B . . 109.5 ?
C7 C8 H8C . . 109.5 ?
H8A C8 H8C . . 109.5 ?
H8B C8 H8C . . 109.5 ?
C1 N1 O1 . . 106.1(4) ?
C1 N1 Zn . . 137.5(3) ?
O1 N1 Zn . . 115.0(2) ?
C1 N2 H2A . . 120.0 ?
C1 N2 H2B . . 120.0 ?
H2A N2 H2B . . 120.0 ?
C5 N3 O2 . . 106.0(3) ?
C5 N3 Zn . . 138.1(3) ?
O2 N3 Zn . . 113.1(3) ?
C5 N4 H4E . . 120.5 ?
C5 N4 H4D . . 119.4 ?
H4E N4 H4D . . 120.0 ?
C3 O1 N1 . . 107.4(3) ?
C7 O2 N3 . . 107.1(4) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zn N3 . 2.002(4) yes
Zn N1 . 2.010(4) yes
Zn Cl2 . 2.2344(13) yes
Zn Cl1 . 2.2372(14) yes
C1 N1 . 1.314(6) yes
C1 N2 . 1.335(6) yes
C1 C2 . 1.399(7) yes
C2 C3 . 1.332(7) yes
C2 H2 . 0.9300 ?
C3 O1 . 1.341(5) yes
C3 C4 . 1.485(7) yes
C4 H4A . 0.9600 ?
C4 H4B . 0.9600 ?
C4 H4C . 0.9600 ?
C5 N3 . 1.306(6) yes
C5 N4 . 1.348(6) yes
C5 C6 . 1.397(7) yes
C6 C7 . 1.325(6) yes
C6 H6 . 0.9300 ?
C7 O2 . 1.348(5) yes
C7 C8 . 1.484(6) yes
C8 H8A . 0.9600 ?
C8 H8B . 0.9600 ?
C8 H8C . 0.9600 ?
N1 O1 . 1.417(4) yes
N2 H2A . 0.8600 ?
N2 H2B . 0.8600 ?
N3 O2 . 1.412(4) yes
N4 H4E . 0.8600 ?
N4 H4D . 0.8600 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N2 H2A Cl2 . 0.86 2.61 3.394(5) 151.2 yes
N4 H4E Cl2 . 0.86 2.67 3.409(4) 144.6 yes
N2 H2B Cl1 3 0.86 2.90 3.341(4) 113.9 yes
N4 H4D Cl1 4_575 0.86 2.72 3.462(4) 145.8 yes
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N1 C1 C2 C3 . . . . -1.3(5) ?
N2 C1 C2 C3 . . . . 179.0(4) ?
C1 C2 C3 O1 . . . . 1.1(5) ?
C1 C2 C3 C4 . . . . 179.8(5) ?
N3 C5 C6 C7 . . . . -2.3(5) ?
N4 C5 C6 C7 . . . . 178.8(5) ?
C5 C6 C7 O2 . . . . 2.4(5) ?
C5 C6 C7 C8 . . . . -176.3(6) ?
N2 C1 N1 O1 . . . . -179.3(4) ?
C2 C1 N1 O1 . . . . 1.0(5) ?
N2 C1 N1 Zn . . . . 15.8(7) ?
C2 C1 N1 Zn . . . . -164.0(4) ?
N3 Zn N1 C1 . . . . -132.6(5) ?
Cl2 Zn N1 C1 . . . . -17.3(5) ?
Cl1 Zn N1 C1 . . . . 112.8(5) ?
N3 Zn N1 O1 . . . . 63.3(3) ?
Cl2 Zn N1 O1 . . . . 178.7(3) ?
Cl1 Zn N1 O1 . . . . -51.3(3) ?
N4 C5 N3 O2 . . . . -179.8(4) ?
C6 C5 N3 O2 . . . . 1.2(5) ?
N4 C5 N3 Zn . . . . -21.3(7) ?
C6 C5 N3 Zn . . . . 159.7(4) ?
N1 Zn N3 C5 . . . . 130.2(5) ?
Cl2 Zn N3 C5 . . . . 14.8(5) ?
Cl1 Zn N3 C5 . . . . -113.5(5) ?
N1 Zn N3 O2 . . . . -72.4(3) ?
Cl2 Zn N3 O2 . . . . 172.2(3) ?
Cl1 Zn N3 O2 . . . . 43.9(3) ?
C2 C3 O1 N1 . . . . -0.5(5) ?
C4 C3 O1 N1 . . . . -179.5(4) ?
C1 N1 O1 C3 . . . . -0.3(5) ?
Zn N1 O1 C3 . . . . 168.6(3) ?
C6 C7 O2 N3 . . . . -1.7(5) ?
C8 C7 O2 N3 . . . . 177.2(4) ?
C5 N3 O2 C7 . . . . 0.2(5) ?
Zn N3 O2 C7 . . . . -164.3(3) ?