#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:38:37 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180347 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/16/7201606.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_7201606
loop_
_publ_author_name
'Yue, Yan-Feng'
'Gao, En-Qing'
'Fang, Chen-Jie'
'Zheng, Tao'
'Liang, Jue'
'Yan, Chun-Hua'
_publ_section_title
;
 The crystal structures of four azido-bridged Zn(ii) complexes based on
 open-chain diazine Schiff-base ligands
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              614
_journal_paper_doi               10.1039/b711831g
_journal_volume                  10
_journal_year                    2008
_chemical_formula_sum            'C12 H13 N15 O Zn2'
_chemical_formula_weight         514.11
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.8350(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5173(3)
_cell_length_b                   10.0830(3)
_cell_length_c                   19.5632(7)
_cell_measurement_reflns_used    16391
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.103
_cell_measurement_theta_min      3.395
_cell_volume                     1851.18(10)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.76
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'NONIUS KappaCCD Diffractometer'
_diffrn_measurement_method       CCD
_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  0.1348
_diffrn_reflns_av_sigmaI/netI    0.1383
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30027
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         3.53
_exptl_absorpt_coefficient_mu    2.635
_exptl_absorpt_correction_T_max  0.907
_exptl_absorpt_correction_T_min  0.689
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            'Light yellow'
_exptl_crystal_density_diffrn    1.845
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.880
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         3905
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.886
_refine_ls_R_factor_all          0.1297
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0446P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0973
_reflns_number_gt                1869
_reflns_number_total             3905
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b711831g.txt
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7201606
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
C1 C 0.5429(5) 0.2063(5) 0.1544(3) 0.0593(15) Uani 1 1 d . . .
H1A H 0.5982 0.2206 0.1290 0.071 Uiso 1 1 calc R . .
C2 C 0.5807(5) 0.2684(6) 0.2235(3) 0.0666(16) Uani 1 1 d . . .
H2A H 0.6604 0.3231 0.2448 0.080 Uiso 1 1 calc R . .
C3 C 0.4981(6) 0.2478(6) 0.2599(3) 0.0719(17) Uani 1 1 d . . .
H3A H 0.5207 0.2899 0.3063 0.086 Uiso 1 1 calc R . .
C4 C 0.3826(5) 0.1656(5) 0.2287(3) 0.0597(15) Uani 1 1 d . . .
H4A H 0.3268 0.1509 0.2537 0.072 Uiso 1 1 calc R . .
C5 C 0.3499(5) 0.1050(5) 0.1596(2) 0.0424(12) Uani 1 1 d . . .
C6 C 0.2287(4) 0.0108(4) 0.1226(2) 0.0382(11) Uani 1 1 d . . .
C7 C 0.0871(5) -0.2233(5) -0.0219(3) 0.0449(12) Uani 1 1 d . . .
C8 C -0.0410(4) -0.3104(5) -0.0433(3) 0.0457(12) Uani 1 1 d . . .
C9 C -0.0872(5) -0.3995(6) -0.1038(3) 0.0604(15) Uani 1 1 d . . .
H9A H -0.0391 -0.4071 -0.1335 0.072 Uiso 1 1 calc R . .
C10 C -0.2045(6) -0.4763(6) -0.1191(4) 0.0713(16) Uani 1 1 d . . .
H10B H -0.2378 -0.5361 -0.1596 0.086 Uiso 1 1 calc R . .
C11 C -0.2724(5) -0.4633(6) -0.0734(3) 0.0676(16) Uani 1 1 d . . .
H11A H -0.3519 -0.5147 -0.0824 0.081 Uiso 1 1 calc R . .
C12 C -0.2205(5) -0.3729(5) -0.0142(3) 0.0608(15) Uani 1 1 d . . .
H12A H -0.2662 -0.3653 0.0167 0.073 Uiso 1 1 calc R . .
N1 N 0.4301(4) 0.1263(4) 0.1222(2) 0.0429(10) Uani 1 1 d . . .
N2 N 0.2286(4) -0.0590(4) 0.0637(2) 0.0406(10) Uani 1 1 d . . .
N3 N 0.1131(4) -0.1448(4) 0.0360(2) 0.0423(10) Uani 1 1 d . . .
N4 N -0.1080(4) -0.2959(4) 0.0009(2) 0.0462(10) Uani 1 1 d . . .
N5 N 0.1328(4) -0.0045(4) 0.1483(2) 0.0514(11) Uani 1 1 d . . .
N6 N 0.1625(4) -0.2351(4) -0.0616(2) 0.0644(13) Uani 1 1 d . . .
N7 N 0.2035(3) 0.0827(4) -0.07990(19) 0.0425(10) Uani 1 1 d . . .
N8 N 0.2227(4) 0.0715(5) -0.1372(3) 0.0611(12) Uani 1 1 d . . .
N9 N 0.2421(6) 0.0623(7) -0.1896(3) 0.109(2) Uani 1 1 d . . .
N10 N 0.4739(4) -0.1288(4) 0.0081(2) 0.0444(10) Uani 1 1 d . . .
N11 N 0.5038(5) -0.2323(6) 0.0421(3) 0.0614(13) Uani 1 1 d . . .
N12 N 0.5341(6) -0.3318(6) 0.0745(4) 0.105(2) Uani 1 1 d . . .
N13 N 0.0450(6) -0.2863(6) 0.1812(3) 0.0843(18) Uani 1 1 d D . .
N14 N -0.004(2) -0.316(3) 0.2172(14) 0.083(6) Uani 0.60(4) 1 d PD A 1
N14' N -0.037(2) -0.359(2) 0.183(2) 0.086(9) Uani 0.40(4) 1 d PD A 2
N15 N -0.059(4) -0.343(4) 0.253(3) 0.25(2) Uani 0.60(4) 1 d PD A 1
N15' N -0.105(2) -0.428(3) 0.1982(17) 0.109(12) Uani 0.40(4) 1 d PD A 2
OW O -0.1661(11) -0.6103(16) 0.1787(6) 0.360(7) Uani 1 1 d . . .
Zn1 Zn 0.36295(5) 0.02422(6) 0.02123(3) 0.04320(19) Uani 1 1 d . . .
Zn2 Zn -0.00813(5) -0.15449(6) 0.09580(3) 0.0475(2) 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 0.0033 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'
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
N1 C1 C2 122.6(5) . . ?
C3 C2 C1 118.3(5) . . ?
C2 C3 C4 120.4(5) . . ?
C3 C4 C5 119.1(4) . . ?
N1 C5 C4 121.1(4) . . ?
N1 C5 C6 116.2(4) . . ?
C4 C5 C6 122.7(4) . . ?
N5 C6 N2 123.8(4) . . ?
N5 C6 C5 121.4(4) . . ?
N2 C6 C5 114.7(4) . . ?
N3 C7 N6 127.5(4) . . ?
N3 C7 C8 114.0(4) . . ?
N6 C7 C8 118.5(4) . . ?
N4 C8 C9 122.3(4) . . ?
N4 C8 C7 114.9(4) . . ?
C9 C8 C7 122.8(4) . . ?
C10 C9 C8 119.1(5) . . ?
C9 C10 C11 118.9(5) . . ?
C10 C11 C12 118.9(5) . . ?
N4 C12 C11 123.1(5) . . ?
C1 N1 C5 118.5(4) . . ?
C1 N1 Zn1 127.1(3) . . ?
C5 N1 Zn1 114.3(3) . . ?
C6 N2 N3 108.7(3) . . ?
C6 N2 Zn1 112.7(3) . . ?
N3 N2 Zn1 135.9(3) . . ?
C7 N3 N2 121.4(3) . . ?
C7 N3 Zn2 121.1(3) . . ?
N2 N3 Zn2 117.4(3) . . ?
C12 N4 C8 117.6(4) . . ?
C12 N4 Zn2 127.1(3) . . ?
C8 N4 Zn2 115.1(3) . . ?
C6 N5 Zn2 113.6(3) . . ?
N8 N7 Zn1 117.4(3) . . ?
N8 N7 Zn2 117.1(3) . 3 ?
Zn1 N7 Zn2 125.41(16) . 3 ?
N9 N8 N7 179.1(6) . . ?
N11 N10 Zn1 128.0(3) . . ?
N11 N10 Zn1 119.9(3) . 3_655 ?
Zn1 N10 Zn1 102.74(18) . 3_655 ?
N12 N11 N10 179.0(5) . . ?
N14 N13 N14' 38.3(10) . . ?
N14 N13 Zn2 133.2(10) . . ?
N14' N13 Zn2 121.4(17) . . ?
N13 N14 N15 178(2) . . ?
N15' N14' N13 169(4) . . ?
N7 Zn1 N10 111.75(16) . . ?
N7 Zn1 N1 124.76(15) . . ?
N10 Zn1 N1 122.58(15) . . ?
N7 Zn1 N2 95.41(13) . . ?
N10 Zn1 N2 105.92(15) . . ?
N1 Zn1 N2 79.66(14) . . ?
N7 Zn1 N10 90.26(14) . 3_655 ?
N10 Zn1 N10 77.26(18) . 3_655 ?
N1 Zn1 N10 92.26(14) . 3_655 ?
N2 Zn1 N10 171.82(14) . 3_655 ?
N13 Zn2 N5 101.9(2) . . ?
N13 Zn2 N7 104.00(17) . 3 ?
N5 Zn2 N7 105.25(15) . 3 ?
N13 Zn2 N3 119.14(17) . . ?
N5 Zn2 N3 76.03(14) . . ?
N7 Zn2 N3 135.85(14) 3 . ?
N13 Zn2 N4 97.0(2) . . ?
N5 Zn2 N4 150.27(13) . . ?
N7 Zn2 N4 92.08(14) 3 . ?
N3 Zn2 N4 74.74(14) . . ?
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
C1 N1 1.334(6) . ?
C1 C2 1.376(6) . ?
C2 C3 1.365(7) . ?
C3 C4 1.366(7) . ?
C4 C5 1.378(6) . ?
C5 N1 1.360(5) . ?
C5 C6 1.489(6) . ?
C6 N5 1.323(5) . ?
C6 N2 1.350(5) . ?
C7 N3 1.306(5) . ?
C7 N6 1.343(5) . ?
C7 C8 1.501(6) . ?
C8 N4 1.349(5) . ?
C8 C9 1.387(6) . ?
C9 C10 1.371(7) . ?
C10 C11 1.379(7) . ?
C11 C12 1.379(7) . ?
C12 N4 1.332(6) . ?
N1 Zn1 2.050(3) . ?
N2 N3 1.387(5) . ?
N2 Zn1 2.110(3) . ?
N3 Zn2 2.085(3) . ?
N4 Zn2 2.196(4) . ?
N5 Zn2 2.041(4) . ?
N7 N8 1.230(5) . ?
N7 Zn1 2.019(3) . ?
N7 Zn2 2.066(3) 3 ?
N8 N9 1.137(5) . ?
N10 N11 1.200(6) . ?
N10 Zn1 2.020(4) . ?
N10 Zn1 2.297(4) 3_655 ?
N11 N12 1.152(6) . ?
N13 N14 1.089(8) . ?
N13 N14' 1.143(10) . ?
N13 Zn2 2.007(5) . ?
N14 N15 1.116(8) . ?
N14' N15' 1.132(10) . ?
Zn1 N10 2.297(4) 3_655 ?
Zn2 N7 2.066(3) 3 ?
